data_nyholmite
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Al0.04 As2.98 Ca0.02 Cd2.89 Cu0.44 Mn0.52 O20 P1.02 Pb0.04 Zn1.05'
_chemical_formula_weight          1035.02
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'As'  'As'   0.0499   2.0058
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cd'  'Cd'  -0.8075   1.2024
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn'  'Zn'   0.2839   1.4301
 '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'
 
_symmetry_cell_setting            'monoclinic'
_symmetry_space_group_name_H-M    'P 1 21/c 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    18.062(4)
_cell_length_b                    9.3410(19)
_cell_length_c                    9.844(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  96.17(3)
_cell_angle_gamma                 90.00
_cell_volume                      1651.2(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     4.498
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2034
_exptl_absorpt_coefficient_mu     14.671
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             8668
_diffrn_reflns_av_R_equivalents   0.0484
_diffrn_reflns_av_sigmaI/netI     0.0444
_diffrn_reflns_limit_h_min        -25
_diffrn_reflns_limit_h_max        25
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.46
_diffrn_reflns_theta_max          30.35
_reflns_number_total              2127
_reflns_number_gt                 2045
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+6.2500P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          2127
_refine_ls_number_parameters      138
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0397
_refine_ls_R_factor_gt            0.0352
_refine_ls_wR_factor_ref          0.0878
_refine_ls_wR_factor_gt           0.0856
_refine_ls_goodness_of_fit_ref    1.081
_refine_ls_restrained_S_all       1.081
_refine_ls_shift/su_max           0.104
_refine_ls_shift/su_mean          0.005
 
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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Cd1 Cd 0.0000 -0.10841(7) 0.2500 0.0175(2) Uani 0.73 2 d SP . .
Zn1 Zn 0.0000 -0.10841(7) 0.2500 0.0175(2) Uani 0.27 2 d SP . .
Zn2 Zn 0.31675(3) 0.08528(6) 0.68609(6) 0.0182(2) Uani 0.31 1 d P . .
Cd2 Cd 0.31675(3) 0.08528(6) 0.68609(6) 0.0182(2) Uani 0.19 1 d P . .
Cu2 Cu 0.31675(3) 0.08528(6) 0.68609(6) 0.0182(2) Uani 0.22 1 d P . .
Mn2 Mn 0.31675(3) 0.08528(6) 0.68609(6) 0.0182(2) Uani 0.26 1 d P . .
Al2 Al 0.31675(3) 0.08528(6) 0.68609(6) 0.0182(2) Uani 0.02 1 d P . .
Cd3 Cd 0.17497(2) 0.02915(4) 0.36559(5) 0.01747(15) Uani 0.89 1 d P . .
Zn3 Zn 0.17497(2) 0.02915(4) 0.36559(5) 0.01747(15) Uani 0.08 1 d P . .
Ca3 Ca 0.17497(2) 0.02915(4) 0.36559(5) 0.01747(15) Uani 0.01 1 d P . .
Pb3 Pb 0.17497(4) 0.02914(7) 0.36562(7) 0.02023(19) Uani 0.02 1 d P . .
As1 As 0.08304(3) 0.18437(6) 0.08980(7) 0.0132(2) Uani 0.66 1 d P . .
P1 P 0.08304(3) 0.18437(6) 0.08980(7) 0.0132(2) Uani 0.34 1 d P . .
As2 As 0.16130(3) 0.26691(6) 0.62386(6) 0.01329(19) Uani 0.83 1 d P . .
P2 P 0.16130(3) 0.26691(6) 0.62386(6) 0.01329(19) Uani 0.17 1 d P . .
O1 O 0.1589(2) 0.2739(5) 0.1355(5) 0.0256(9) Uani 1 1 d . . .
O2 O 0.0109(3) 0.2965(5) 0.0791(5) 0.0310(10) Uani 1 1 d . . .
O3 O 0.0756(2) 0.0658(5) 0.2090(5) 0.0270(10) Uani 1 1 d . . .
O4 O 0.0840(2) 0.1110(5) -0.0616(4) 0.0261(9) Uani 1 1 d . . .
O5 O 0.1656(2) 0.2488(4) 0.4541(4) 0.0231(9) Uani 1 1 d . . .
O6 O 0.0725(2) 0.2749(4) 0.6556(5) 0.0241(9) Uani 1 1 d . . .
O7 O 0.2054(2) 0.4159(4) 0.6779(4) 0.0215(9) Uani 1 1 d . . .
O8 O 0.2048(2) 0.1280(4) 0.7023(5) 0.0246(9) Uani 1 1 d . . .
O9 O 0.4177(3) -0.0034(5) 0.6614(6) 0.0363(12) Uani 1 1 d . . .
O10 O 0.2604(2) -0.0840(4) 0.5323(4) 0.0240(9) Uani 1 1 d . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Cd1 0.0182(4) 0.0127(3) 0.0213(4) 0.000 0.0008(2) 0.000
Zn1 1.9(12) 0.11(10) 2.0(14) 0.000 -0.4(10) 0.000
Zn2 0.0215(3) 0.0108(3) 0.0219(4) 0.0034(2) 0.0008(2) -0.0004(2)
Cd3 0.0182(2) 0.0126(2) 0.0217(3) -0.00237(15) 0.00225(16) -0.00114(14)
As1 0.0148(3) 0.0096(3) 0.0150(4) -0.0009(2) 0.0006(2) 0.0015(2)
P1 0.0148(3) 0.0096(3) 0.0150(4) -0.0009(2) 0.0006(2) 0.0015(2)
As2 0.0149(3) 0.0070(3) 0.0173(3) -0.00036(19) -0.0012(2) 0.00044(18)
P2 0.0149(3) 0.0070(3) 0.0173(3) -0.00036(19) -0.0012(2) 0.00044(18)
O1 0.024(2) 0.025(2) 0.027(2) -0.0025(17) 0.0004(17) -0.0045(16)
O2 0.035(2) 0.029(2) 0.028(2) -0.0087(18) -0.0015(19) 0.0082(18)
O3 0.025(2) 0.022(2) 0.034(3) 0.0083(18) 0.0011(18) -0.0034(16)
O4 0.024(2) 0.030(2) 0.024(2) -0.0047(17) 0.0021(17) 0.0103(17)
O5 0.029(2) 0.0182(18) 0.021(2) -0.0039(15) -0.0023(16) 0.0015(15)
O6 0.0205(19) 0.0175(18) 0.033(2) -0.0018(17) -0.0009(17) 0.0000(15)
O7 0.0193(18) 0.0157(17) 0.031(2) -0.0024(15) 0.0085(16) -0.0018(14)
O8 0.024(2) 0.0143(17) 0.036(2) 0.0075(16) 0.0051(17) 0.0018(15)
O9 0.033(3) 0.032(2) 0.044(3) 0.015(2) 0.003(2) -0.0081(19)
O10 0.026(2) 0.0220(19) 0.025(2) 0.0045(16) 0.0076(16) 0.0018(16)
 
_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
Cd1 O3 2.192(4) 2 ?
Cd1 O3 2.192(4) . ?
Cd1 O4 2.267(4) 5 ?
Cd1 O4 2.267(4) 6_556 ?
Cd1 O6 2.293(4) 5_556 ?
Cd1 O6 2.293(4) 6 ?
Zn2 O9 2.039(5) . ?
Zn2 O8 2.084(4) . ?
Zn2 O5 2.121(4) 7_556 ?
Zn2 O7 2.138(4) 4_546 ?
Zn2 O1 2.200(4) 7_556 ?
Zn2 O10 2.345(5) . ?
Cd3 O5 2.244(4) . ?
Cd3 O3 2.265(5) . ?
Cd3 O4 2.277(4) 6_556 ?
Cd3 O8 2.285(4) 6 ?
Cd3 O7 2.305(4) 7_556 ?
Cd3 O10 2.377(4) . ?
As1 O1 1.626(4) . ?
As1 O3 1.627(4) . ?
As1 O4 1.641(4) . ?
As1 O2 1.666(5) . ?
As2 O8 1.663(4) . ?
As2 O7 1.663(4) . ?
As2 O6 1.669(4) . ?
As2 O5 1.689(4) . ?
O1 Zn2 2.200(4) 7_556 ?
O4 Zn1 2.267(4) 5 ?
O4 Cd1 2.267(4) 5 ?
O4 Cd3 2.277(4) 6 ?
O5 Zn2 2.121(4) 7_556 ?
O6 Zn1 2.293(4) 5_556 ?
O6 Cd1 2.293(4) 5_556 ?
O7 Zn2 2.138(4) 4_556 ?
O7 Cd3 2.305(4) 7_556 ?
O8 Cd3 2.285(4) 6_556 ?
 
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
O3 Cd1 O3 83.7(2) 2 . ?
O3 Cd1 O4 77.54(16) 2 5 ?
O3 Cd1 O4 103.44(17) . 5 ?
O3 Cd1 O4 103.44(17) 2 6_556 ?
O3 Cd1 O4 77.54(16) . 6_556 ?
O4 Cd1 O4 178.7(2) 5 6_556 ?
O3 Cd1 O6 92.11(16) 2 5_556 ?
O3 Cd1 O6 166.72(17) . 5_556 ?
O4 Cd1 O6 87.88(16) 5 5_556 ?
O4 Cd1 O6 91.25(15) 6_556 5_556 ?
O3 Cd1 O6 166.72(17) 2 6 ?
O3 Cd1 O6 92.11(16) . 6 ?
O4 Cd1 O6 91.25(15) 5 6 ?
O4 Cd1 O6 87.88(16) 6_556 6 ?
O6 Cd1 O6 94.6(2) 5_556 6 ?
O9 Zn2 O8 166.80(18) . . ?
O9 Zn2 O5 91.14(18) . 7_556 ?
O8 Zn2 O5 97.15(16) . 7_556 ?
O9 Zn2 O7 90.26(17) . 4_546 ?
O8 Zn2 O7 81.10(16) . 4_546 ?
O5 Zn2 O7 177.51(17) 7_556 4_546 ?
O9 Zn2 O1 103.49(19) . 7_556 ?
O8 Zn2 O1 86.38(17) . 7_556 ?
O5 Zn2 O1 92.96(16) 7_556 7_556 ?
O7 Zn2 O1 88.71(17) 4_546 7_556 ?
O9 Zn2 O10 88.86(18) . . ?
O8 Zn2 O10 79.73(16) . . ?
O5 Zn2 O10 99.06(15) 7_556 . ?
O7 Zn2 O10 78.92(16) 4_546 . ?
O1 Zn2 O10 162.62(15) 7_556 . ?
O5 Cd3 O3 92.11(16) . . ?
O5 Cd3 O4 108.48(16) . 6_556 ?
O3 Cd3 O4 75.88(15) . 6_556 ?
O5 Cd3 O8 153.50(15) . 6 ?
O3 Cd3 O8 81.35(17) . 6 ?
O4 Cd3 O8 94.87(16) 6_556 6 ?
O5 Cd3 O7 88.85(15) . 7_556 ?
O3 Cd3 O7 122.03(16) . 7_556 ?
O4 Cd3 O7 155.38(15) 6_556 7_556 ?
O8 Cd3 O7 73.46(14) 6 7_556 ?
O5 Cd3 O10 102.09(15) . . ?
O3 Cd3 O10 161.24(15) . . ?
O4 Cd3 O10 87.91(15) 6_556 . ?
O8 Cd3 O10 90.85(15) 6 . ?
O7 Cd3 O10 71.04(15) 7_556 . ?
O1 As1 O3 106.4(2) . . ?
O1 As1 O4 112.0(2) . . ?
O3 As1 O4 112.5(2) . . ?
O1 As1 O2 108.9(2) . . ?
O3 As1 O2 110.3(2) . . ?
O4 As1 O2 106.8(2) . . ?
O8 As2 O7 108.5(2) . . ?
O8 As2 O6 111.3(2) . . ?
O7 As2 O6 109.9(2) . . ?
O8 As2 O5 108.2(2) . . ?
O7 As2 O5 109.2(2) . . ?
O6 As2 O5 109.7(2) . . ?
As1 O1 Zn2 128.2(2) . 7_556 ?
As1 O3 Cd1 137.7(3) . . ?
As1 O3 Cd3 118.2(2) . . ?
Cd1 O3 Cd3 102.97(17) . . ?
As1 O4 Zn1 132.6(2) . 5 ?
As1 O4 Cd1 132.6(2) . 5 ?
Zn1 O4 Cd1 0 5 5 ?
As1 O4 Cd3 127.2(2) . 6 ?
Zn1 O4 Cd3 100.23(17) 5 6 ?
Cd1 O4 Cd3 100.23(17) 5 6 ?
As2 O5 Zn2 126.7(2) . 7_556 ?
As2 O5 Cd3 119.2(2) . . ?
Zn2 O5 Cd3 113.10(19) 7_556 . ?
As2 O6 Zn1 130.4(2) . 5_556 ?
As2 O6 Cd1 130.4(2) . 5_556 ?
Zn1 O6 Cd1 0.00(2) 5_556 5_556 ?
As2 O7 Zn2 134.8(2) . 4_556 ?
As2 O7 Cd3 123.6(2) . 7_556 ?
Zn2 O7 Cd3 101.21(16) 4_556 7_556 ?
As2 O8 Zn2 121.9(2) . . ?
As2 O8 Cd3 133.8(2) . 6_556 ?
Zn2 O8 Cd3 103.58(17) . 6_556 ?
Zn2 O10 Cd3 110.49(17) . . ?
 
_diffrn_measured_fraction_theta_max    0.858
_diffrn_reflns_theta_full              30.35
_diffrn_measured_fraction_theta_full   0.858
_refine_diff_density_max    1.492
_refine_diff_density_min   -0.894
_refine_diff_density_rms    0.221