# Datablock #1

data_Nickolayite_Holotype
# The type material

_chemical_name_mineral             'Nickolayite'
_chemical_compound_source          'Transjordan Plateau, West Jordan'
_chemical_formula_analytical       'Fe1.02 Mo0.87 Ni0.11 P1.02'
_chemical_formula_sum              'Fe Mo0.88 Ni0.12 P'
_chemical_formula_weight           178.29

loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mo' 'Mo' -1.6832 0.6857
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system        'orthorhombic'
_space_group_IT_number             62
_space_group_name_H-M_alt          'P n m a'
_space_group_name_Hall             '-P 2ac 2n'

loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'

_cell_length_a                     5.9519(5)
_cell_length_b                     3.7070(3)
_cell_length_c                     6.8465(6)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       151.06(2)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      3683
_cell_measurement_temperature      296(2)
_cell_measurement_theta_max        39.8770
_cell_measurement_theta_min        3.0230
_exptl_absorpt_coefficient_mu      18.770
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.57377
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour              'grey'
_exptl_crystal_density_diffrn      7.840
_exptl_crystal_density_meas        .
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         block
_exptl_crystal_F_000               325
_exptl_crystal_size_max            0.06
_exptl_crystal_size_mid            0.06
_exptl_crystal_size_min            0.04
_diffrn_reflns_av_R_equivalents    0.0374
_diffrn_reflns_av_unetI/netI       0.0113
_diffrn_reflns_Laue_measured_fraction_full  0.994
_diffrn_reflns_Laue_measured_fraction_max  0.996
_diffrn_reflns_limit_h_max         8
_diffrn_reflns_limit_h_min         -8
_diffrn_reflns_limit_k_max         5
_diffrn_reflns_limit_k_min         -5
_diffrn_reflns_limit_l_max         9
_diffrn_reflns_limit_l_min         -9
_diffrn_reflns_number              3338
_diffrn_reflns_point_group_measured_fraction_full  0.994
_diffrn_reflns_point_group_measured_fraction_max  0.996
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           29.875
_diffrn_reflns_theta_min           4.538
_diffrn_ambient_temperature        296(2)
_diffrn_detector                   'CCD plate'
_diffrn_measured_fraction_theta_full  0.994
_diffrn_measured_fraction_theta_max  0.996

_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  φ   -360.00   1.00   1.00   30.00  13.03 -38.00  64.00    --   361
  2  ω    246.97 326.97   1.00   30.00    --  -40.00 -33.99  -2.00   80
  3  ω    -80.07 -34.07   1.00   30.00    --  -42.00  96.00  78.00   46
  4  ω    234.50 341.50   1.00   30.00    --  -42.00 -37.99-174.00  107
  5  φ   -360.00   1.00   1.00   30.00 -23.53 -42.00 -56.01    --   361
  6  φ   -360.00   1.00   1.00   30.00 -63.68 -42.00  66.00    --   361
;

_diffrn_measurement_device         'Bruker Kappa APEX DUO CCD'
_diffrn_measurement_device_type     'four-circle diffractometer' 
_diffrn_measurement_method         'ω and φ scans'
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Mo K\a'
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'fine-focus sealed X-ray tube'
_diffrn_source_type                'Enhance (Mo) X-ray Source'
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  251
_reflns_number_total               251
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'Bruker APEX2'
_computing_data_collection         'Bruker APEX2'
_computing_data_reduction          'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics      'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2018 (Sheldrick, 2015)'
_refine_diff_density_max           0.971
_refine_diff_density_min           -0.994
_refine_diff_density_rms           0.222
_refine_ls_extinction_coef         0.007(2)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.136
_refine_ls_matrix_type             full
_refine_ls_number_parameters       20
_refine_ls_number_reflns           251
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0174
_refine_ls_R_factor_gt             0.0174
_refine_ls_restrained_S_all        1.136
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0255P)²+0.5924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0435
_refine_ls_wR_factor_ref           0.0435

_refine_special_details
;
1. Shared sites
{Mo1, Ni1}
2. Uiso/Uaniso restraints and constraints
Uanis(Mo1) = Uanis(Ni1)
3. Others
 Fixed Sof: Mo1(0.44) Ni1(0.06)
;

_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     difmap

loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Mo1 Mo 0.02900(5) 0.750000 0.67160(5) 0.00459(17) Uani 0.88 2 d S T P . .
 Ni1 Ni 0.02900(5) 0.750000 0.67160(5) 0.00459(17) Uani 0.12 2 d S T P . .
 Fe2 Fe 0.64102(9) 0.750000 0.43729(8) 0.00477(18) Uani 1 2 d S T P . .
 P1 P 0.26587(16) 0.750000 0.37739(15) 0.0057(2) Uani 1 2 d S T P . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Mo1 Mo1 3.0126(5) 5_566 ?
 Mo1 Fe2 2.7595(7) 6_557 ?
 Mo1 Fe2 2.8015(5) 5_666 ?
 Mo1 Fe2 2.8118(7) 1_455 ?
 Mo1 Fe2 2.7871(5) 2_565 ?
 Mo1 Fe2 2.8015(5) 5_676 ?
 Mo1 Fe2 2.7871(5) 2_575 ?
 Mo1 P1 2.5745(7) 5_566 ?
 Mo1 P1 2.6289(7) 2_565 ?
 Mo1 P1 2.4587(10) . ?
 Mo1 P1 2.5745(7) 5_576 ?
 Mo1 P1 2.6289(7) 2_575 ?
 Fe2 Fe2 2.6440(8) 5_666 ?
 Fe2 Fe2 2.6440(8) 5_676 ?
 Fe2 P1 2.3136(7) 5_676 ?
 Fe2 P1 2.2790(11) 6_656 ?
 Fe2 P1 2.3136(7) 5_666 ?
 Fe2 P1 2.2702(11) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 Fe2 Mo1 Mo1 93.341(12) 2_565 5_566 ?
 Fe2 Mo1 Mo1 57.376(13) 1_455 5_566 ?
 Fe2 Mo1 Mo1 106.251(18) 5_676 5_566 ?
 Fe2 Mo1 Mo1 57.707(13) 5_666 5_566 ?
 Fe2 Mo1 Mo1 141.679(9) 6_557 5_566 ?
 Fe2 Mo1 Mo1 151.23(2) 2_575 5_566 ?
 Fe2 Mo1 Fe2 150.25(2) 2_575 5_666 ?
 Fe2 Mo1 Fe2 83.367(18) 2_575 2_565 ?
 Fe2 Mo1 Fe2 115.082(15) 5_676 1_455 ?
 Fe2 Mo1 Fe2 95.097(13) 6_557 5_676 ?
 Fe2 Mo1 Fe2 94.254(11) 2_565 1_455 ?
 Fe2 Mo1 Fe2 89.325(13) 2_575 5_676 ?
 Fe2 Mo1 Fe2 115.082(15) 5_666 1_455 ?
 Fe2 Mo1 Fe2 56.936(15) 6_557 2_565 ?
 Fe2 Mo1 Fe2 94.254(11) 2_575 1_455 ?
 Fe2 Mo1 Fe2 89.325(13) 2_565 5_666 ?
 Fe2 Mo1 Fe2 150.25(2) 2_565 5_676 ?
 Fe2 Mo1 Fe2 82.845(18) 5_676 5_666 ?
 Fe2 Mo1 Fe2 95.097(13) 6_557 5_666 ?
 Fe2 Mo1 Fe2 138.77(2) 6_557 1_455 ?
 Fe2 Mo1 Fe2 56.936(15) 6_557 2_575 ?
 P1 Mo1 Mo1 154.82(3) 2_575 5_566 ?
 P1 Mo1 Mo1 51.49(2) 5_566 5_566 ?
 P1 Mo1 Mo1 105.26(3) 5_576 5_566 ?
 P1 Mo1 Mo1 92.146(19) 2_565 5_566 ?
 P1 Mo1 Mo1 55.020(18) . 5_566 ?
 P1 Mo1 Fe2 51.684(16) . 5_676 ?
 P1 Mo1 Fe2 133.407(17) 2_575 1_455 ?
 P1 Mo1 Fe2 106.93(3) 5_576 6_557 ?
 P1 Mo1 Fe2 108.44(2) 5_576 2_565 ?
 P1 Mo1 Fe2 131.03(3) . 6_557 ?
 P1 Mo1 Fe2 137.977(10) . 2_565 ?
 P1 Mo1 Fe2 50.11(2) 5_566 2_565 ?
 P1 Mo1 Fe2 50.11(2) 5_576 2_575 ?
 P1 Mo1 Fe2 106.72(2) 2_575 2_565 ?
 P1 Mo1 Fe2 137.977(10) . 2_575 ?
 P1 Mo1 Fe2 49.46(2) 2_565 2_565 ?
 P1 Mo1 Fe2 50.640(19) 5_576 1_455 ?
 P1 Mo1 Fe2 49.50(2) 2_575 5_676 ?
 P1 Mo1 Fe2 133.407(17) 2_565 1_455 ?
 P1 Mo1 Fe2 106.47(2) 2_565 5_676 ?
 P1 Mo1 Fe2 106.93(3) 5_566 6_557 ?
 P1 Mo1 Fe2 51.684(16) . 5_666 ?
 P1 Mo1 Fe2 50.78(2) 2_575 6_557 ?
 P1 Mo1 Fe2 88.10(2) 5_566 5_666 ?
 P1 Mo1 Fe2 156.86(3) 5_566 5_676 ?
 P1 Mo1 Fe2 156.86(3) 5_576 5_666 ?
 P1 Mo1 Fe2 88.10(2) 5_576 5_676 ?
 P1 Mo1 Fe2 106.47(2) 2_575 5_666 ?
 P1 Mo1 Fe2 50.783(19) 2_565 6_557 ?
 P1 Mo1 Fe2 49.50(2) 2_565 5_666 ?
 P1 Mo1 Fe2 108.44(2) 5_566 2_575 ?
 P1 Mo1 Fe2 90.20(3) . 1_455 ?
 P1 Mo1 Fe2 106.72(2) 2_565 2_575 ?
 P1 Mo1 Fe2 50.640(19) 5_566 1_455 ?
 P1 Mo1 Fe2 49.46(2) 2_575 2_575 ?
 P1 Mo1 P1 106.51(3) . 5_566 ?
 P1 Mo1 P1 153.38(2) 5_576 2_565 ?
 P1 Mo1 P1 99.950(13) . 2_565 ?
 P1 Mo1 P1 92.10(3) 5_566 5_576 ?
 P1 Mo1 P1 83.040(18) 5_576 2_575 ?
 P1 Mo1 P1 99.950(13) . 2_575 ?
 P1 Mo1 P1 83.040(18) 5_566 2_565 ?
 P1 Mo1 P1 153.38(2) 5_566 2_575 ?
 P1 Mo1 P1 89.67(3) 2_575 2_565 ?
 P1 Mo1 P1 106.51(3) . 5_576 ?
 Mo1 Fe2 Mo1 123.064(15) 6_657 2_564 ?
 Mo1 Fe2 Mo1 68.954(10) 2_564 5_666 ?
 Mo1 Fe2 Mo1 132.109(12) 2_574 1_655 ?
 Mo1 Fe2 Mo1 132.109(12) 2_564 1_655 ?
 Mo1 Fe2 Mo1 82.845(18) 5_676 5_666 ?
 Mo1 Fe2 Mo1 83.367(18) 2_564 2_574 ?
 Mo1 Fe2 Mo1 115.315(17) 6_657 5_666 ?
 Mo1 Fe2 Mo1 64.918(15) 5_666 1_655 ?
 Mo1 Fe2 Mo1 121.39(2) 2_574 5_666 ?
 Mo1 Fe2 Mo1 115.315(17) 6_657 5_676 ?
 Mo1 Fe2 Mo1 69.193(14) 6_657 1_655 ?
 Mo1 Fe2 Mo1 121.39(2) 2_564 5_676 ?
 Mo1 Fe2 Mo1 68.954(10) 2_574 5_676 ?
 Mo1 Fe2 Mo1 64.917(15) 5_676 1_655 ?
 Mo1 Fe2 Mo1 123.064(15) 6_657 2_574 ?
 Fe2 Fe2 Mo1 116.59(3) 5_666 2_574 ?
 Fe2 Fe2 Mo1 93.883(12) 5_666 5_666 ?
 Fe2 Fe2 Mo1 109.64(3) 5_666 1_655 ?
 Fe2 Fe2 Mo1 61.006(17) 5_676 2_574 ?
 Fe2 Fe2 Mo1 61.006(17) 5_666 2_564 ?
 Fe2 Fe2 Mo1 109.64(3) 5_676 1_655 ?
 Fe2 Fe2 Mo1 116.59(3) 5_676 2_564 ?
 Fe2 Fe2 Mo1 174.45(3) 5_666 5_676 ?
 Fe2 Fe2 Mo1 174.45(3) 5_676 5_666 ?
 Fe2 Fe2 Mo1 93.883(12) 5_676 5_676 ?
 Fe2 Fe2 Mo1 62.06(2) 5_666 6_657 ?
 Fe2 Fe2 Mo1 62.06(2) 5_676 6_657 ?
 Fe2 Fe2 Fe2 89.02(3) 5_666 5_676 ?
 P1 Fe2 Mo1 174.95(4) 6_656 6_657 ?
 P1 Fe2 Mo1 167.87(3) 5_666 2_574 ?
 P1 Fe2 Mo1 59.36(2) 5_676 1_655 ?
 P1 Fe2 Mo1 167.87(3) 5_676 2_564 ?
 P1 Fe2 Mo1 120.53(3) 5_666 5_676 ?
 P1 Fe2 Mo1 105.76(3) 6_656 1_655 ?
 P1 Fe2 Mo1 59.36(2) 5_666 1_655 ?
 P1 Fe2 Mo1 60.09(2) 6_656 2_564 ?
 P1 Fe2 Mo1 61.69(3) 5_666 6_657 ?
 P1 Fe2 Mo1 84.96(2) 5_666 2_564 ?
 P1 Fe2 Mo1 60.09(2) 6_656 2_574 ?
 P1 Fe2 Mo1 155.62(4) . 1_655 ?
 P1 Fe2 Mo1 56.49(2) 5_666 5_666 ?
 P1 Fe2 Mo1 86.43(3) . 6_657 ?
 P1 Fe2 Mo1 84.96(2) 5_676 2_574 ?
 P1 Fe2 Mo1 61.30(2) 6_656 5_676 ?
 P1 Fe2 Mo1 61.64(2) . 2_564 ?
 P1 Fe2 Mo1 56.49(2) 5_676 5_676 ?
 P1 Fe2 Mo1 129.900(19) . 5_666 ?
 P1 Fe2 Mo1 61.64(2) . 2_574 ?
 P1 Fe2 Mo1 61.30(2) 6_656 5_666 ?
 P1 Fe2 Mo1 120.53(3) 5_676 5_666 ?
 P1 Fe2 Mo1 129.900(19) . 5_676 ?
 P1 Fe2 Mo1 61.69(3) 5_676 6_657 ?
 P1 Fe2 Fe2 120.94(3) 6_656 5_666 ?
 P1 Fe2 Fe2 120.94(3) 6_656 5_676 ?
 P1 Fe2 Fe2 55.54(2) . 5_666 ?
 P1 Fe2 Fe2 122.38(4) 5_676 5_666 ?
 P1 Fe2 Fe2 54.01(3) 5_676 5_676 ?
 P1 Fe2 Fe2 54.01(3) 5_666 5_666 ?
 P1 Fe2 Fe2 55.54(2) . 5_676 ?
 P1 Fe2 Fe2 122.38(4) 5_666 5_676 ?
 P1 Fe2 P1 109.55(3) . 5_676 ?
 P1 Fe2 P1 98.62(3) . 6_656 ?
 P1 Fe2 P1 106.48(5) 5_676 5_666 ?
 P1 Fe2 P1 116.13(2) 6_656 5_676 ?
 P1 Fe2 P1 116.13(2) 6_656 5_666 ?
 P1 Fe2 P1 109.55(3) . 5_666 ?
 Mo1 P1 Mo1 89.67(3) 2_564 2_574 ?
 Mo1 P1 Mo1 138.97(4) 5_576 2_564 ?
 Mo1 P1 Mo1 134.860(17) . 2_564 ?
 Mo1 P1 Mo1 134.860(17) . 2_574 ?
 Mo1 P1 Mo1 92.10(3) 5_566 5_576 ?
 Mo1 P1 Mo1 74.881(14) 5_576 2_574 ?
 Mo1 P1 Mo1 74.881(14) 5_566 2_564 ?
 Mo1 P1 Mo1 73.49(3) . 5_566 ?
 Mo1 P1 Mo1 73.49(3) . 5_576 ?
 Mo1 P1 Mo1 138.97(4) 5_566 2_574 ?
 Fe2 P1 Mo1 69.79(3) 6_556 5_576 ?
 Fe2 P1 Mo1 133.950(16) . 5_576 ?
 Fe2 P1 Mo1 68.90(2) . 2_574 ?
 Fe2 P1 Mo1 69.999(17) 5_676 5_576 ?
 Fe2 P1 Mo1 71.82(3) 5_676 . ?
 Fe2 P1 Mo1 144.24(4) 5_666 5_576 ?
 Fe2 P1 Mo1 67.533(18) 5_676 2_574 ?
 Fe2 P1 Mo1 114.58(4) . . ?
 Fe2 P1 Mo1 125.98(4) 6_556 . ?
 Fe2 P1 Mo1 69.79(3) 6_556 5_566 ?
 Fe2 P1 Mo1 71.82(3) 5_666 . ?
 Fe2 P1 Mo1 68.90(2) . 2_564 ?
 Fe2 P1 Mo1 69.19(3) 6_556 2_574 ?
 Fe2 P1 Mo1 69.19(3) 6_556 2_564 ?
 Fe2 P1 Mo1 138.38(4) 5_666 2_574 ?
 Fe2 P1 Mo1 138.38(4) 5_676 2_564 ?
 Fe2 P1 Mo1 67.533(18) 5_666 2_564 ?
 Fe2 P1 Mo1 144.24(4) 5_676 5_566 ?
 Fe2 P1 Mo1 69.999(17) 5_666 5_566 ?
 Fe2 P1 Mo1 133.950(16) . 5_566 ?
 Fe2 P1 Fe2 119.44(5) . 6_556 ?
 Fe2 P1 Fe2 126.62(2) 6_556 5_666 ?
 Fe2 P1 Fe2 70.45(3) . 5_666 ?
 Fe2 P1 Fe2 70.45(3) . 5_676 ?
 Fe2 P1 Fe2 106.48(5) 5_676 5_666 ?
 Fe2 P1 Fe2 126.62(2) 6_556 5_676 ?


# End of datablock Nickolayite_Holotype


# Datablock #2
data_Nickolayite_low_Mo

_chemical_name_mineral             'Nickolayite'
_chemical_compound_source          'Transjordan Plateau, West Jordan'
_chemical_formula_sum              'Fe1.45 Mo0.45 Ni0.10 P'
_chemical_formula_analytical       'Co0.01 Fe1.44 Mo0.44 Ni0.10 P1.01'
_chemical_formula_weight           161.00


loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mo' 'Mo' -1.6832 0.6857
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system        'orthorhombic'
_space_group_IT_number             62
_space_group_name_H-M_alt          'P n m a'
_space_group_name_Hall             '-P 2ac 2n'

loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'

_cell_length_a                     5.8544(6)
_cell_length_b                     3.6241(4)
_cell_length_c                     6.7182(7)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       142.54(3)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      763
_cell_measurement_temperature      296(2)
_cell_measurement_theta_max        31.7440
_cell_measurement_theta_min        4.5950
_exptl_absorpt_coefficient_mu      20.422
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.04896
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.86a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour              'grey'
_exptl_crystal_density_diffrn      7.502
_exptl_crystal_density_meas        .
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         block
_exptl_crystal_F_000               298
_exptl_crystal_size_max            0.05
_exptl_crystal_size_mid            0.05
_exptl_crystal_size_min            0.03
_diffrn_reflns_av_R_equivalents    0.0275
_diffrn_reflns_av_unetI/netI       0.0240
_diffrn_reflns_Laue_measured_fraction_full  0.993
_diffrn_reflns_Laue_measured_fraction_max  0.983
_diffrn_reflns_limit_h_max         8
_diffrn_reflns_limit_h_min         -8
_diffrn_reflns_limit_k_max         4
_diffrn_reflns_limit_k_min         -4
_diffrn_reflns_limit_l_max         5
_diffrn_reflns_limit_l_min         -9
_diffrn_reflns_number              952
_diffrn_reflns_point_group_measured_fraction_full  0.993
_diffrn_reflns_point_group_measured_fraction_max  0.983
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           29.917
_diffrn_reflns_theta_min           4.618
_diffrn_ambient_temperature        296(2)
_diffrn_detector                   'CCD plate'
_diffrn_measured_fraction_theta_full  0.993
_diffrn_measured_fraction_theta_max  0.983

_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     -9.79 179.21   1.00  380.00    --   20.00  73.86  19.21  189
  2  φ   -212.82 -16.66   1.00  379.96  96.71 -22.50  73.86    --   196
;
_diffrn_measurement_device       'Bruker APEX II CCD'
_diffrn_measurement_device_type  'two-circle diffractometer'
_diffrn_measurement_method         'ω and φ scans'
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Mo K\a'
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'fine-focus sealed X-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  205
_reflns_number_total               235
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'Bruker APEX2'
_computing_data_collection         'Bruker APEX2'
_computing_data_reduction          'CrysAlisPro 1.171.41.86a (Rigaku OD, 2020)'
_computing_molecular_graphics      'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2018 (Sheldrick, 2015)'
_refine_diff_density_max           1.164
_refine_diff_density_min           -1.200
_refine_diff_density_rms           0.273
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.144
_refine_ls_hydrogen_treatment      undef
_refine_ls_matrix_type             full
_refine_ls_number_parameters       19
_refine_ls_number_reflns           235
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0293
_refine_ls_R_factor_gt             0.0224
_refine_ls_restrained_S_all        1.144
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0203P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0402
_refine_ls_wR_factor_ref           0.0415
_refine_special_details
;
1. Shared sites
{Mo1, Fe1, Ni1}
2. Uiso/Uaniso restraints and constraints
Uanis(Mo1) = Uanis(Fe1) = Uanis(Ni1)
3. Others
 Fixed Sof: Mo1(0.225) Fe1(0.225) Ni1(0.05)
;

_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     difmap

loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Mo1 Mo 0.02847(9) 0.750000 0.66915(8) 0.00469(16) Uani 0.45 2 d S T P . .
 Fe1 Fe 0.02847(9) 0.750000 0.66915(8) 0.00469(16) Uani 0.45 2 d S T P . .
 Ni1 Ni 0.02847(9) 0.750000 0.66915(8) 0.00469(16) Uani 0.1 2 d S T P . .
 Fe2 Fe 0.64222(12) 0.750000 0.43740(11) 0.00451(19) Uani 1 2 d S T P . .
 P1 P 0.2640(2) 0.750000 0.37652(19) 0.0053(3) Uani 1 2 d S T P . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Mo1 Mo1 2.9258(9) 5_566 ?
 Mo1 Fe2 2.7258(9) 6_557 ?
 Mo1 Fe2 2.7441(7) 2_565 ?
 Mo1 Fe2 2.7454(9) 1_455 ?
 Mo1 Fe2 2.7410(7) 5_666 ?
 Mo1 Fe2 2.7441(7) 2_575 ?
 Mo1 Fe2 2.7410(7) 5_676 ?
 Mo1 P1 2.5118(10) 5_566 ?
 Mo1 P1 2.5886(10) 2_565 ?
 Mo1 P1 2.4013(15) . ?
 Mo1 P1 2.5118(10) 5_576 ?
 Mo1 P1 2.5886(10) 2_575 ?
 Fe2 Fe2 2.6007(10) 5_666 ?
 Fe2 Fe2 2.6007(10) 5_676 ?
 Fe2 P1 2.2689(9) 5_676 ?
 Fe2 P1 2.2518(15) . ?
 Fe2 P1 2.2689(9) 5_666 ?
 Fe2 P1 2.2262(15) 6_656 ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 Fe2 Mo1 Mo1 57.85(2) 5_666 5_566 ?
 Fe2 Mo1 Mo1 57.70(2) 1_455 5_566 ?
 Fe2 Mo1 Mo1 151.36(3) 2_575 5_566 ?
 Fe2 Mo1 Mo1 93.423(17) 2_565 5_566 ?
 Fe2 Mo1 Mo1 141.362(14) 6_557 5_566 ?
 Fe2 Mo1 Mo1 106.66(3) 5_676 5_566 ?
 Fe2 Mo1 Fe2 149.79(3) 5_676 2_565 ?
 Fe2 Mo1 Fe2 82.77(3) 5_676 5_666 ?
 Fe2 Mo1 Fe2 94.158(16) 2_575 1_455 ?
 Fe2 Mo1 Fe2 56.78(2) 6_557 2_575 ?
 Fe2 Mo1 Fe2 115.55(2) 5_666 1_455 ?
 Fe2 Mo1 Fe2 89.490(17) 5_676 2_575 ?
 Fe2 Mo1 Fe2 94.158(16) 2_565 1_455 ?
 Fe2 Mo1 Fe2 94.670(19) 6_557 5_666 ?
 Fe2 Mo1 Fe2 115.55(2) 5_676 1_455 ?
 Fe2 Mo1 Fe2 89.490(17) 5_666 2_565 ?
 Fe2 Mo1 Fe2 149.79(3) 5_666 2_575 ?
 Fe2 Mo1 Fe2 82.65(3) 2_575 2_565 ?
 Fe2 Mo1 Fe2 56.78(2) 6_557 2_565 ?
 Fe2 Mo1 Fe2 138.69(3) 6_557 1_455 ?
 Fe2 Mo1 Fe2 94.670(19) 6_557 5_676 ?
 P1 Mo1 Mo1 154.84(4) 2_575 5_566 ?
 P1 Mo1 Mo1 51.73(3) 5_566 5_566 ?
 P1 Mo1 Mo1 105.92(3) 5_576 5_566 ?
 P1 Mo1 Mo1 92.18(2) 2_565 5_566 ?
 P1 Mo1 Mo1 55.21(3) . 5_566 ?
 P1 Mo1 Fe2 138.313(14) . 2_575 ?
 P1 Mo1 Fe2 133.77(2) 2_575 1_455 ?
 P1 Mo1 Fe2 106.56(3) 5_576 6_557 ?
 P1 Mo1 Fe2 157.59(4) 5_576 5_666 ?
 P1 Mo1 Fe2 130.82(4) . 6_557 ?
 P1 Mo1 Fe2 51.85(3) . 5_666 ?
 P1 Mo1 Fe2 88.32(3) 5_566 5_666 ?
 P1 Mo1 Fe2 88.32(3) 5_576 5_676 ?
 P1 Mo1 Fe2 105.85(3) 2_575 5_666 ?
 P1 Mo1 Fe2 51.85(3) . 5_676 ?
 P1 Mo1 Fe2 49.28(3) 2_565 5_666 ?
 P1 Mo1 Fe2 50.90(3) 5_576 1_455 ?
 P1 Mo1 Fe2 49.85(3) 2_575 2_575 ?
 P1 Mo1 Fe2 133.77(2) 2_565 1_455 ?
 P1 Mo1 Fe2 106.24(4) 2_565 2_575 ?
 P1 Mo1 Fe2 106.56(3) 5_566 6_557 ?
 P1 Mo1 Fe2 138.313(14) . 2_565 ?
 P1 Mo1 Fe2 50.47(3) 2_575 6_557 ?
 P1 Mo1 Fe2 49.88(3) 5_566 2_565 ?
 P1 Mo1 Fe2 107.96(3) 5_566 2_575 ?
 P1 Mo1 Fe2 107.96(3) 5_576 2_565 ?
 P1 Mo1 Fe2 49.88(3) 5_576 2_575 ?
 P1 Mo1 Fe2 106.24(4) 2_575 2_565 ?
 P1 Mo1 Fe2 50.47(3) 2_565 6_557 ?
 P1 Mo1 Fe2 49.85(3) 2_565 2_565 ?
 P1 Mo1 Fe2 157.59(4) 5_566 5_676 ?
 P1 Mo1 Fe2 90.50(4) . 1_455 ?
 P1 Mo1 Fe2 105.85(3) 2_565 5_676 ?
 P1 Mo1 Fe2 50.90(3) 5_566 1_455 ?
 P1 Mo1 Fe2 49.28(3) 2_575 5_676 ?
 P1 Mo1 P1 106.94(4) . 5_566 ?
 P1 Mo1 P1 152.96(4) 5_576 2_565 ?
 P1 Mo1 P1 99.851(18) . 2_565 ?
 P1 Mo1 P1 92.34(5) 5_566 5_576 ?
 P1 Mo1 P1 83.15(2) 5_576 2_575 ?
 P1 Mo1 P1 99.851(18) . 2_575 ?
 P1 Mo1 P1 83.15(2) 5_566 2_565 ?
 P1 Mo1 P1 152.96(4) 5_566 2_575 ?
 P1 Mo1 P1 88.86(4) 2_575 2_565 ?
 P1 Mo1 P1 106.94(4) . 5_576 ?
 Mo1 Fe2 Mo1 115.16(2) 6_657 5_676 ?
 Mo1 Fe2 Mo1 69.394(14) 5_676 2_574 ?
 Mo1 Fe2 Mo1 64.45(2) 5_666 1_655 ?
 Mo1 Fe2 Mo1 64.45(2) 5_676 1_655 ?
 Mo1 Fe2 Mo1 82.65(3) 2_564 2_574 ?
 Mo1 Fe2 Mo1 82.77(3) 5_676 5_666 ?
 Mo1 Fe2 Mo1 123.22(2) 6_657 2_574 ?
 Mo1 Fe2 Mo1 132.251(17) 2_574 1_655 ?
 Mo1 Fe2 Mo1 121.41(3) 5_666 2_574 ?
 Mo1 Fe2 Mo1 123.22(2) 6_657 2_564 ?
 Mo1 Fe2 Mo1 69.59(2) 6_657 1_655 ?
 Mo1 Fe2 Mo1 121.41(3) 5_676 2_564 ?
 Mo1 Fe2 Mo1 69.394(13) 5_666 2_564 ?
 Mo1 Fe2 Mo1 132.251(17) 2_564 1_655 ?
 Mo1 Fe2 Mo1 115.16(2) 6_657 5_666 ?
 Fe2 Fe2 Mo1 94.255(16) 5_666 5_666 ?
 Fe2 Fe2 Mo1 116.06(4) 5_666 2_574 ?
 Fe2 Fe2 Mo1 110.12(4) 5_666 1_655 ?
 Fe2 Fe2 Mo1 174.52(4) 5_676 5_666 ?
 Fe2 Fe2 Mo1 174.52(4) 5_666 5_676 ?
 Fe2 Fe2 Mo1 110.12(4) 5_676 1_655 ?
 Fe2 Fe2 Mo1 94.255(16) 5_676 5_676 ?
 Fe2 Fe2 Mo1 61.26(2) 5_666 2_564 ?
 Fe2 Fe2 Mo1 61.26(2) 5_676 2_574 ?
 Fe2 Fe2 Mo1 116.06(4) 5_676 2_564 ?
 Fe2 Fe2 Mo1 61.96(3) 5_666 6_657 ?
 Fe2 Fe2 Mo1 61.96(3) 5_676 6_657 ?
 Fe2 Fe2 Fe2 88.33(4) 5_666 5_676 ?
 P1 Fe2 Mo1 86.33(4) . 6_657 ?
 P1 Fe2 Mo1 56.34(4) 5_666 5_666 ?
 P1 Fe2 Mo1 59.22(3) 5_676 1_655 ?
 P1 Fe2 Mo1 56.34(4) 5_676 5_676 ?
 P1 Fe2 Mo1 85.56(3) 5_666 2_564 ?
 P1 Fe2 Mo1 155.92(5) . 1_655 ?
 P1 Fe2 Mo1 59.22(3) 5_666 1_655 ?
 P1 Fe2 Mo1 130.11(3) . 5_676 ?
 P1 Fe2 Mo1 61.63(4) 5_666 6_657 ?
 P1 Fe2 Mo1 120.11(4) 5_666 5_676 ?
 P1 Fe2 Mo1 130.11(3) . 5_666 ?
 P1 Fe2 Mo1 105.87(5) 6_656 1_655 ?
 P1 Fe2 Mo1 167.79(4) 5_666 2_574 ?
 P1 Fe2 Mo1 175.46(5) 6_656 6_657 ?
 P1 Fe2 Mo1 120.11(4) 5_676 5_666 ?
 P1 Fe2 Mo1 61.48(3) . 2_564 ?
 P1 Fe2 Mo1 61.79(3) 6_656 5_676 ?
 P1 Fe2 Mo1 167.79(4) 5_676 2_564 ?
 P1 Fe2 Mo1 59.63(3) 6_656 2_574 ?
 P1 Fe2 Mo1 61.79(3) 6_656 5_666 ?
 P1 Fe2 Mo1 61.48(3) . 2_574 ?
 P1 Fe2 Mo1 85.56(3) 5_676 2_574 ?
 P1 Fe2 Mo1 59.63(3) 6_656 2_564 ?
 P1 Fe2 Mo1 61.63(4) 5_676 6_657 ?
 P1 Fe2 Fe2 55.19(3) . 5_666 ?
 P1 Fe2 Fe2 55.19(3) . 5_676 ?
 P1 Fe2 Fe2 120.76(4) 6_656 5_666 ?
 P1 Fe2 Fe2 122.22(6) 5_676 5_666 ?
 P1 Fe2 Fe2 54.57(4) 5_676 5_676 ?
 P1 Fe2 Fe2 54.57(4) 5_666 5_666 ?
 P1 Fe2 Fe2 120.76(4) 6_656 5_676 ?
 P1 Fe2 Fe2 122.22(6) 5_666 5_676 ?
 P1 Fe2 P1 116.39(3) 6_656 5_676 ?
 P1 Fe2 P1 98.21(4) 6_656 . ?
 P1 Fe2 P1 106.00(6) 5_676 5_666 ?
 P1 Fe2 P1 109.76(4) . 5_676 ?
 P1 Fe2 P1 109.76(4) . 5_666 ?
 P1 Fe2 P1 116.39(3) 6_656 5_666 ?
 Mo1 P1 Mo1 88.86(4) 2_564 2_574 ?
 Mo1 P1 Mo1 139.40(5) 5_576 2_564 ?
 Mo1 P1 Mo1 135.25(2) . 2_564 ?
 Mo1 P1 Mo1 135.25(2) . 2_574 ?
 Mo1 P1 Mo1 92.34(5) 5_566 5_576 ?
 Mo1 P1 Mo1 75.476(18) 5_576 2_574 ?
 Mo1 P1 Mo1 75.476(18) 5_566 2_564 ?
 Mo1 P1 Mo1 73.06(4) . 5_566 ?
 Mo1 P1 Mo1 73.06(4) . 5_576 ?
 Mo1 P1 Mo1 139.40(5) 5_566 2_574 ?
 Fe2 P1 Mo1 133.83(2) . 5_576 ?
 Fe2 P1 Mo1 70.49(4) 6_556 5_576 ?
 Fe2 P1 Mo1 68.93(4) 6_556 2_574 ?
 Fe2 P1 Mo1 69.89(2) 5_676 5_576 ?
 Fe2 P1 Mo1 71.81(4) 5_676 . ?
 Fe2 P1 Mo1 143.94(6) 5_666 5_576 ?
 Fe2 P1 Mo1 67.90(3) 5_676 2_574 ?
 Fe2 P1 Mo1 126.28(7) 6_556 . ?
 Fe2 P1 Mo1 114.58(6) . . ?
 Fe2 P1 Mo1 133.83(2) . 5_566 ?
 Fe2 P1 Mo1 71.81(4) 5_666 . ?
 Fe2 P1 Mo1 68.93(4) 6_556 2_564 ?
 Fe2 P1 Mo1 68.66(4) . 2_574 ?
 Fe2 P1 Mo1 68.66(4) . 2_564 ?
 Fe2 P1 Mo1 137.90(6) 5_666 2_574 ?
 Fe2 P1 Mo1 137.90(6) 5_676 2_564 ?
 Fe2 P1 Mo1 67.90(3) 5_666 2_564 ?
 Fe2 P1 Mo1 143.94(6) 5_676 5_566 ?
 Fe2 P1 Mo1 69.89(2) 5_666 5_566 ?
 Fe2 P1 Mo1 70.49(4) 6_556 5_566 ?
 Fe2 P1 Fe2 119.14(6) 6_556 . ?
 Fe2 P1 Fe2 70.24(4) . 5_666 ?
 Fe2 P1 Fe2 126.83(3) 6_556 5_666 ?
 Fe2 P1 Fe2 126.83(3) 6_556 5_676 ?
 Fe2 P1 Fe2 106.00(6) 5_676 5_666 ?
 Fe2 P1 Fe2 70.24(4) . 5_676 ?


# End of datablock Nickolayite_low_Mo