#============================================================================== data_New_Global_Publ_Block _audit_update_record ; 2015-12-14 # Formatted by publCIF ; # publcif _publ_body_element loop start loop_ _publ_body_element _publ_body_title _publ_body_contents section ; Introduction ; ; ; section ; Experimental ; ; ; subsection ; Synthesis and crystallization ; ; ; subsection ; Refinement ; ; Crystal data, data collection and structure refinement details are summarized in Table 1. ; section ; Results and discussion ; ; ; # publcif _publ_body_element loop end # Added by publCIF - use a unique identifier for each data block #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'M.B. ANDRADE' # Name of author for correspondence _publ_contact_author_address # Address of author for correspondence ; Department of Physics and Interdisciplinary Science, Sao Carlos Institute of Physics, University of Sao Paulo, Caixa Postal 369, Sao Carlos, SP, 13560-970, Brazil ; _publ_contact_author_email 'mabadean@terra.com.br' _publ_contact_author_fax '+55-16-33739881' _publ_contact_author_phone '+55-16-33738096' _publ_contact_letter ; Please consider this CIF for publication. I certify that this contibution is the original work of those listed as authors; that it has not been published before (in any language or medium) and is not being considered for publication elsewhere; that all authors concur with and are aware of the submission; that all workers involved in the study are listed as authors or given proper credit in the acknowledgements; that I have obtained permission for and acknowledged the source of any excerpts from other copyright works; and that to the best of my knowledge the paper contains no statements which are libellous, unlawful or in any way actionable. All coauthors have made significant scientific contributions to the work reported, including the ideas and their execution, and share responsibility and accountability for the results. ; _publ_requested_journal 'Mineralogical Magazine' _publ_requested_category FI #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Hydroxycalciomicrolite, Ca~1.5~Ta~2~O~6~(OH), a new member of the microlite group from Volta Grande pegmatite, Nazareno, Minas Gerais, Brazil ; _publ_section_title_footnote # remove if not required . # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # NB if using publCIF, the Author database tool might prove useful # (see the Tools menu in publCIF) loop_ _publ_author_name _publ_author_address _publ_author_footnote _publ_author_email 'ANDRADE, M.B.' ; Department of Physics and Interdisciplinary Science, Sao Carlos Institute of Physics, University of Sao Paulo, Caixa Postal 369, Sao Carlos, SP, 13560-970,Brazil ; ? ; mabadean@terra.com.br ; 'YANG, H.' ; Department of Geosciences, University of Arizona, 1040 E. 4th Street, Tucson, Arizona 85721-0077, USA ; . ; hyang@u.arizona.edu ; 'ATENCIO, D.' ; Departamento de Mineralogia e Geotect\^onica, Instituto de Geoci\^encias, Universidade de S\~ao Paulo, Rua do Lago, 562, 05508-080 S\~ao Paulo, SP, Brazil ; . ; datencio@usp.br ; 'DOWNS, R.T.' ; Department of Geosciences, University of Arizona, 1040 E. 4th Street, Tucson, Arizona 85721-0077, USA ; . ; rdowns@u.arizona.edu ; 'CHUKANOV, N.V.' ; Institute of Problems of Chemical Physics, Russian Academy of Sciences, Chernogolovka, Moscow Region 142432, Russia ; . ; chukanov@icp.ac.ru ; 'Lem\'ee-Cailleau, M.H.' ; Institut Laue Langevin (ILL), 6 Rue Jules Horowitz, BP 156 38042, Grenoble, France ; . ; lemee@ill.eu ; 'PERSIANO, A.I.C.' ; Departamento de F\'isica, Universidade Federal de Minas Gerais, Avenida Presidente Antonio Carlos 6627, 30123-970, Belo Horizonte, MG, Brazil ; . ; persiano@fisica.ufmg.br ; 'GOETA, A.E.' ; Department of Chemistry, Durham University, Durham, UK DH1 3LE ; . . 'ELLENA, J.' ; Department of Physics and Interdisciplinary Science, Sao Carlos Institute of Physics, University of Sao Paulo, Caixa Postal 369, Sao Carlos, SP, 13560-970, Brazil ; . ; javiere@ifsc.usp.br ; #============================================================================== # TEXT _publ_section_synopsis . _publ_section_abstract ; (type here to add) ; _publ_section_acknowledgements # remove if not required ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ; #============================================================================== data_amab _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_mineral 'hydroxycalciomicrolite' _chemical_compound_source 'Volta Grande pegmatite, Nazareno, Minas Gerais, Brazil' _chemical_formula_moiety '(Ca1.46 Na0.15) (Ta1.72 Nb0.28) O6 ((O H)0.65 F0.35))' _chemical_formula_sum 'Ca1.46 F0.35 H0.65 Na0.15 Nb0.28 O6.65 Ta1.72' _chemical_formula_weight 512.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ta' 'Ta' -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system cubic _space_group_IT_number 212 _symmetry_space_group_name_H-M 'P 43 3 2' _symmetry_space_group_name_Hall 'P 4acd 2ab 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'y+3/4, -x+3/4, z+1/4' '-y+3/4, x+1/4, z+3/4' 'x+1/4, z+3/4, -y+3/4' '-x+3/4, z+1/4, y+3/4' '-x+1/4, -z+1/4, -y+1/4' 'x+3/4, -z+3/4, y+1/4' 'z+1/4, y+3/4, -x+3/4' 'z+3/4, -y+3/4, x+1/4' '-z+3/4, y+1/4, x+3/4' '-z+1/4, -y+1/4, -x+1/4' _cell_length_a 10.42050(10) _cell_length_b 10.42050(10) _cell_length_c 10.42050(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1131.529(19) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1085 _cell_measurement_theta_min 5.524 _cell_measurement_theta_max 68.873 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.020 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1799 _exptl_absorpt_coefficient_mu 35.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2728 _exptl_absorpt_correction_T_max 0.5404 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2005)' _exptl_special_details ? _diffrn_ambient_temperature 296(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 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6086 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 33.72 _reflns_number_total 749 _reflns_number_gt 497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'publCIF (Westrip, 2010)' _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^)+(0.0000P)^2^+26.4419P] 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 SHELXL _refine_ls_extinction_coef 0.00129(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 256 Friedel pairs' _refine_ls_abs_structure_Flack 0.7(4) _refine_ls_number_reflns 749 _refine_ls_number_parameters 35 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ta2 Ta 0.3750 0.37388(2) 0.12388(2) 0.00421(16) Uani 0.86(2) 2 d SP . . Nb2 Nb 0.3750 0.37388(2) 0.12388(2) 0.00421(16) Uani 0.14(2) 2 d SP . . Ta1 Ta 0.1250 0.1250 0.1250 0.0044(2) Uani 0.86(2) 6 d SP . . Nb1 Nb 0.1250 0.1250 0.1250 0.0044(2) Uani 0.14(2) 6 d SP . . Ca1 Ca 0.62174(15) 0.37174(15) 0.3750 0.0155(7) Uani 0.972(19) 2 d SP . . Na1 Na 0.6250 0.6250 0.6250 0.008(2) Uiso 0.31(3) 6 d SP . . O3 O 0.2517(5) 0.0592(5) 0.2482(6) 0.0124(11) Uiso 1 1 d . . . O2 O 0.4447(5) 0.2507(5) 0.2506(5) 0.0103(10) Uiso 1 1 d . . . F1 F 0.481(3) 0.481(3) 0.481(3) 0.016(8) Uiso 0.35(9) 3 d SP . . O1 O 0.5046(14) 0.5046(14) 0.5046(14) 0.001(4) Uiso 0.65(9) 3 d SPD . . H1 H 0.5538(18) 0.5538(18) 0.5538(18) 0.030 Uiso 0.7(4) 3 d SPD . . 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 Ta2 0.0042(2) 0.00422(17) 0.00422(17) 0.00172(12) 0.00020(11) -0.00020(11) Nb2 0.0042(2) 0.00422(17) 0.00422(17) 0.00172(12) 0.00020(11) -0.00020(11) Ta1 0.0044(2) 0.0044(2) 0.0044(2) -0.00014(19) -0.00014(19) -0.00014(19) Nb1 0.0044(2) 0.0044(2) 0.0044(2) -0.00014(19) -0.00014(19) -0.00014(19) Ca1 0.0159(8) 0.0159(8) 0.0146(11) -0.0050(7) 0.0050(7) 0.0045(12) _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 Ta2 O3 1.955(5) 5 ? Ta2 O3 1.955(5) 23_554 ? Ta2 O2 1.979(5) 18_554 ? Ta2 O2 1.979(5) . ? Ta2 O2 1.993(5) 23_554 ? Ta2 O2 1.993(5) 5 ? Ta2 Ca1 3.653(2) 5 ? Ta2 Na1 3.6677(4) 3_645 ? Ta2 Ca1 3.6687(11) . ? Ta2 Ca1 3.6687(11) 12_564 ? Ta2 Ca1 3.7003(12) 7_564 ? Ta2 Ca1 3.7003(12) 8_645 ? Ta1 O3 1.965(6) 24 ? Ta1 O3 1.965(6) 5 ? Ta1 O3 1.965(6) 14 ? Ta1 O3 1.965(6) . ? Ta1 O3 1.965(6) 9 ? Ta1 O3 1.965(6) 19 ? Ta1 Na1 3.6842 3_645 ? Ta1 Na1 3.6842 2_564 ? Ta1 Na1 3.6842 4_456 ? Ta1 Ca1 3.732(2) 7_564 ? Ta1 Ca1 3.732(2) 3_645 ? Ta1 Ca1 3.732(2) 11_456 ? Ca1 F1 2.160(11) 13_545 ? Ca1 F1 2.160(11) . ? Ca1 O1 2.287(10) 13_545 ? Ca1 O1 2.287(10) . ? Ca1 O2 2.583(5) . ? Ca1 O2 2.583(5) 13_545 ? Ca1 O2 2.638(5) 23_554 ? Ca1 O2 2.638(5) 11_556 ? Ca1 O3 2.683(6) 15 ? Ca1 O3 2.683(6) 3_655 ? Ca1 Ta2 3.653(2) 9 ? Ca1 Nb2 3.653(2) 9 ? Ca1 H1 2.75(2) . ? Na1 O1 2.17(3) . ? Na1 O1 2.17(3) 14_666 ? Na1 F1 2.60(5) . ? Na1 F1 2.60(5) 14_666 ? Na1 O3 2.678(6) 15 ? Na1 O3 2.678(6) 8_655 ? Na1 O3 2.678(6) 21 ? Na1 O3 2.678(6) 12_565 ? Na1 O3 2.678(6) 18 ? Na1 O3 2.678(6) 4_556 ? Na1 Ta2 3.6677(4) 3_655 ? Na1 Nb2 3.6677(4) 3_655 ? Na1 H1 1.28(3) . ? O3 Nb2 1.955(5) 9 ? O3 Ta2 1.955(5) 9 ? O3 Na1 2.678(6) 4_456 ? O3 Ca1 2.683(5) 3_645 ? O2 Nb2 1.993(5) 9 ? O2 Ta2 1.993(5) 9 ? O2 Ca1 2.638(5) 8_645 ? F1 Ca1 2.160(11) 5 ? F1 Ca1 2.160(11) 9 ? F1 H1 1.32(4) . ? O1 Ca1 2.287(10) 5 ? O1 Ca1 2.287(10) 9 ? O1 H1 0.89(2) . ? 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 Ta2 O3 90.4(3) 5 23_554 ? O3 Ta2 O2 87.9(2) 5 18_554 ? O3 Ta2 O2 93.2(2) 23_554 18_554 ? O3 Ta2 O2 93.2(2) 5 . ? O3 Ta2 O2 87.9(2) 23_554 . ? O2 Ta2 O2 178.5(3) 18_554 . ? O3 Ta2 O2 177.8(2) 5 23_554 ? O3 Ta2 O2 91.7(2) 23_554 23_554 ? O2 Ta2 O2 92.1(3) 18_554 23_554 ? O2 Ta2 O2 86.79(18) . 23_554 ? O3 Ta2 O2 91.7(2) 5 5 ? O3 Ta2 O2 177.8(2) 23_554 5 ? O2 Ta2 O2 86.79(18) 18_554 5 ? O2 Ta2 O2 92.1(3) . 5 ? O2 Ta2 O2 86.1(3) 23_554 5 ? O3 Ta2 Ca1 134.78(17) 5 5 ? O3 Ta2 Ca1 134.78(17) 23_554 5 ? O2 Ta2 Ca1 89.24(16) 18_554 5 ? O2 Ta2 Ca1 89.24(16) . 5 ? O2 Ta2 Ca1 43.04(15) 23_554 5 ? O2 Ta2 Ca1 43.04(15) 5 5 ? O3 Ta2 Na1 45.22(17) 5 3_645 ? O3 Ta2 Na1 45.22(17) 23_554 3_645 ? O2 Ta2 Na1 90.76(16) 18_554 3_645 ? O2 Ta2 Na1 90.76(16) . 3_645 ? O2 Ta2 Na1 136.96(15) 23_554 3_645 ? O2 Ta2 Na1 136.96(15) 5 3_645 ? Ca1 Ta2 Na1 180.0 5 3_645 ? O3 Ta2 Ca1 135.71(16) 5 . ? O3 Ta2 Ca1 89.35(17) 23_554 . ? O2 Ta2 Ca1 136.37(16) 18_554 . ? O2 Ta2 Ca1 42.52(15) . . ? O2 Ta2 Ca1 44.27(15) 23_554 . ? O2 Ta2 Ca1 89.14(16) 5 . ? Ca1 Ta2 Ca1 59.995(12) 5 . ? Na1 Ta2 Ca1 120.005(12) 3_645 . ? O3 Ta2 Ca1 89.35(17) 5 12_564 ? O3 Ta2 Ca1 135.71(16) 23_554 12_564 ? O2 Ta2 Ca1 42.52(15) 18_554 12_564 ? O2 Ta2 Ca1 136.37(16) . 12_564 ? O2 Ta2 Ca1 89.14(16) 23_554 12_564 ? O2 Ta2 Ca1 44.27(15) 5 12_564 ? Ca1 Ta2 Ca1 59.995(12) 5 12_564 ? Na1 Ta2 Ca1 120.005(12) 3_645 12_564 ? Ca1 Ta2 Ca1 119.99(2) . 12_564 ? O3 Ta2 Ca1 44.53(16) 5 7_564 ? O3 Ta2 Ca1 91.02(17) 23_554 7_564 ? O2 Ta2 Ca1 43.36(16) 18_554 7_564 ? O2 Ta2 Ca1 137.74(15) . 7_564 ? O2 Ta2 Ca1 135.46(15) 23_554 7_564 ? O2 Ta2 Ca1 90.48(16) 5 7_564 ? Ca1 Ta2 Ca1 119.562(10) 5 7_564 ? Na1 Ta2 Ca1 60.438(10) 3_645 7_564 ? Ca1 Ta2 Ca1 179.558(10) . 7_564 ? Ca1 Ta2 Ca1 59.57(2) 12_564 7_564 ? O3 Ta2 Ca1 91.02(17) 5 8_645 ? O3 Ta2 Ca1 44.53(16) 23_554 8_645 ? O2 Ta2 Ca1 137.74(15) 18_554 8_645 ? O2 Ta2 Ca1 43.36(16) . 8_645 ? O2 Ta2 Ca1 90.48(16) 23_554 8_645 ? O2 Ta2 Ca1 135.46(15) 5 8_645 ? Ca1 Ta2 Ca1 119.562(10) 5 8_645 ? Na1 Ta2 Ca1 60.438(10) 3_645 8_645 ? Ca1 Ta2 Ca1 59.57(2) . 8_645 ? Ca1 Ta2 Ca1 179.558(10) 12_564 8_645 ? Ca1 Ta2 Ca1 120.875(19) 7_564 8_645 ? O3 Ta1 O3 87.6(3) 24 5 ? O3 Ta1 O3 91.4(2) 24 14 ? O3 Ta1 O3 89.7(3) 5 14 ? O3 Ta1 O3 178.5(3) 24 . ? O3 Ta1 O3 91.4(2) 5 . ? O3 Ta1 O3 87.6(3) 14 . ? O3 Ta1 O3 89.7(3) 24 9 ? O3 Ta1 O3 91.4(2) 5 9 ? O3 Ta1 O3 178.5(3) 14 9 ? O3 Ta1 O3 91.4(2) . 9 ? O3 Ta1 O3 91.4(2) 24 19 ? O3 Ta1 O3 178.5(3) 5 19 ? O3 Ta1 O3 91.4(2) 14 19 ? O3 Ta1 O3 89.7(3) . 19 ? O3 Ta1 O3 87.6(3) 9 19 ? O3 Ta1 Na1 89.24(17) 24 3_645 ? O3 Ta1 Na1 44.87(17) 5 3_645 ? O3 Ta1 Na1 44.87(17) 14 3_645 ? O3 Ta1 Na1 89.24(17) . 3_645 ? O3 Ta1 Na1 136.22(15) 9 3_645 ? O3 Ta1 Na1 136.22(15) 19 3_645 ? O3 Ta1 Na1 44.87(17) 24 2_564 ? O3 Ta1 Na1 89.24(17) 5 2_564 ? O3 Ta1 Na1 136.22(15) 14 2_564 ? O3 Ta1 Na1 136.22(15) . 2_564 ? O3 Ta1 Na1 44.87(17) 9 2_564 ? O3 Ta1 Na1 89.24(17) 19 2_564 ? Na1 Ta1 Na1 120.0 3_645 2_564 ? O3 Ta1 Na1 136.22(15) 24 4_456 ? O3 Ta1 Na1 136.22(15) 5 4_456 ? O3 Ta1 Na1 89.24(17) 14 4_456 ? O3 Ta1 Na1 44.87(17) . 4_456 ? O3 Ta1 Na1 89.24(17) 9 4_456 ? O3 Ta1 Na1 44.87(17) 19 4_456 ? Na1 Ta1 Na1 120.0 3_645 4_456 ? Na1 Ta1 Na1 120.0 2_564 4_456 ? O3 Ta1 Ca1 43.78(15) 24 7_564 ? O3 Ta1 Ca1 43.78(15) 5 7_564 ? O3 Ta1 Ca1 90.76(17) 14 7_564 ? O3 Ta1 Ca1 135.13(17) . 7_564 ? O3 Ta1 Ca1 90.76(17) 9 7_564 ? O3 Ta1 Ca1 135.13(17) 19 7_564 ? Na1 Ta1 Ca1 60.0 3_645 7_564 ? Na1 Ta1 Ca1 60.0 2_564 7_564 ? Na1 Ta1 Ca1 180.0 4_456 7_564 ? O3 Ta1 Ca1 135.13(17) 24 3_645 ? O3 Ta1 Ca1 90.76(17) 5 3_645 ? O3 Ta1 Ca1 43.78(15) 14 3_645 ? O3 Ta1 Ca1 43.78(15) . 3_645 ? O3 Ta1 Ca1 135.13(17) 9 3_645 ? O3 Ta1 Ca1 90.76(17) 19 3_645 ? Na1 Ta1 Ca1 60.0 3_645 3_645 ? Na1 Ta1 Ca1 180.0 2_564 3_645 ? Na1 Ta1 Ca1 60.0 4_456 3_645 ? Ca1 Ta1 Ca1 120.0 7_564 3_645 ? O3 Ta1 Ca1 90.76(17) 24 11_456 ? O3 Ta1 Ca1 135.13(17) 5 11_456 ? O3 Ta1 Ca1 135.13(17) 14 11_456 ? O3 Ta1 Ca1 90.76(17) . 11_456 ? O3 Ta1 Ca1 43.78(15) 9 11_456 ? O3 Ta1 Ca1 43.78(15) 19 11_456 ? Na1 Ta1 Ca1 180.0 3_645 11_456 ? Na1 Ta1 Ca1 60.0 2_564 11_456 ? Na1 Ta1 Ca1 60.0 4_456 11_456 ? Ca1 Ta1 Ca1 120.0 7_564 11_456 ? Ca1 Ta1 Ca1 120.0 3_645 11_456 ? F1 Ca1 F1 168(2) 13_545 . ? F1 Ca1 O1 10.5(10) 13_545 13_545 ? F1 Ca1 O1 173.8(12) . 13_545 ? F1 Ca1 O1 173.8(12) 13_545 . ? F1 Ca1 O1 10.5(10) . . ? O1 Ca1 O1 174.2(10) 13_545 . ? F1 Ca1 O2 77.8(7) 13_545 . ? F1 Ca1 O2 91.6(14) . . ? O1 Ca1 O2 82.8(3) 13_545 . ? O1 Ca1 O2 102.2(6) . . ? F1 Ca1 O2 91.6(14) 13_545 13_545 ? F1 Ca1 O2 77.8(7) . 13_545 ? O1 Ca1 O2 102.2(6) 13_545 13_545 ? O1 Ca1 O2 82.8(3) . 13_545 ? O2 Ca1 O2 63.6(2) . 13_545 ? F1 Ca1 O2 103.7(7) 13_545 23_554 ? F1 Ca1 O2 76.5(6) . 23_554 ? O1 Ca1 O2 98.3(3) 13_545 23_554 ? O1 Ca1 O2 81.6(3) . 23_554 ? O2 Ca1 O2 63.02(5) . 23_554 ? O2 Ca1 O2 119.0(2) 13_545 23_554 ? F1 Ca1 O2 76.5(6) 13_545 11_556 ? F1 Ca1 O2 103.7(7) . 11_556 ? O1 Ca1 O2 81.6(3) 13_545 11_556 ? O1 Ca1 O2 98.3(3) . 11_556 ? O2 Ca1 O2 119.0(2) . 11_556 ? O2 Ca1 O2 63.02(5) 13_545 11_556 ? O2 Ca1 O2 177.9(3) 23_554 11_556 ? F1 Ca1 O3 101.2(7) 13_545 15 ? F1 Ca1 O3 89.5(14) . 15 ? O1 Ca1 O3 96.0(3) 13_545 15 ? O1 Ca1 O3 79.0(6) . 15 ? O2 Ca1 O3 178.42(19) . 15 ? O2 Ca1 O3 117.78(17) 13_545 15 ? O2 Ca1 O3 116.22(18) 23_554 15 ? O2 Ca1 O3 61.71(17) 11_556 15 ? F1 Ca1 O3 89.5(14) 13_545 3_655 ? F1 Ca1 O3 101.2(7) . 3_655 ? O1 Ca1 O3 79.0(6) 13_545 3_655 ? O1 Ca1 O3 96.0(3) . 3_655 ? O2 Ca1 O3 117.78(17) . 3_655 ? O2 Ca1 O3 178.42(19) 13_545 3_655 ? O2 Ca1 O3 61.71(17) 23_554 3_655 ? O2 Ca1 O3 116.22(18) 11_556 3_655 ? O3 Ca1 O3 60.9(3) 15 3_655 ? F1 Ca1 Ta2 83.8(12) 13_545 9 ? F1 Ca1 Ta2 83.8(12) . 9 ? O1 Ca1 Ta2 92.9(5) 13_545 9 ? O1 Ca1 Ta2 92.9(5) . 9 ? O2 Ca1 Ta2 31.78(12) . 9 ? O2 Ca1 Ta2 31.78(12) 13_545 9 ? O2 Ca1 Ta2 91.07(13) 23_554 9 ? O2 Ca1 Ta2 91.07(13) 11_556 9 ? O3 Ca1 Ta2 149.56(13) 15 9 ? O3 Ca1 Ta2 149.56(13) 3_655 9 ? F1 Ca1 Nb2 83.8(12) 13_545 9 ? F1 Ca1 Nb2 83.8(12) . 9 ? O1 Ca1 Nb2 92.9(5) 13_545 9 ? O1 Ca1 Nb2 92.9(5) . 9 ? O2 Ca1 Nb2 31.78(12) . 9 ? O2 Ca1 Nb2 31.78(12) 13_545 9 ? O2 Ca1 Nb2 91.07(13) 23_554 9 ? O2 Ca1 Nb2 91.07(13) 11_556 9 ? O3 Ca1 Nb2 149.56(13) 15 9 ? O3 Ca1 Nb2 149.56(13) 3_655 9 ? Ta2 Ca1 Nb2 0.000(11) 9 9 ? F1 Ca1 H1 161.8(7) 13_545 . ? F1 Ca1 H1 27.9(11) . . ? O1 Ca1 H1 157.4(8) 13_545 . ? O1 Ca1 H1 17.4(4) . . ? O2 Ca1 H1 119.5(5) . . ? O2 Ca1 H1 91.5(3) 13_545 . ? O2 Ca1 H1 90.4(3) 23_554 . ? O2 Ca1 H1 89.0(3) 11_556 . ? O3 Ca1 H1 61.6(5) 15 . ? O3 Ca1 H1 87.0(3) 3_655 . ? Ta2 Ca1 H1 107.8(4) 9 . ? Nb2 Ca1 H1 107.8(4) 9 . ? O1 Na1 O1 180.0(6) . 14_666 ? O1 Na1 F1 0.0(8) . . ? O1 Na1 F1 180.0(8) 14_666 . ? O1 Na1 F1 180.0(8) . 14_666 ? O1 Na1 F1 0.0(19) 14_666 14_666 ? F1 Na1 F1 180.000(2) . 14_666 ? O1 Na1 O3 81.03(11) . 15 ? O1 Na1 O3 98.97(11) 14_666 15 ? F1 Na1 O3 81.03(11) . 15 ? F1 Na1 O3 98.97(11) 14_666 15 ? O1 Na1 O3 98.97(11) . 8_655 ? O1 Na1 O3 81.03(11) 14_666 8_655 ? F1 Na1 O3 98.97(11) . 8_655 ? F1 Na1 O3 81.03(11) 14_666 8_655 ? O3 Na1 O3 62.3(2) 15 8_655 ? O1 Na1 O3 81.03(11) . 21 ? O1 Na1 O3 98.97(11) 14_666 21 ? F1 Na1 O3 81.03(11) . 21 ? F1 Na1 O3 98.97(11) 14_666 21 ? O3 Na1 O3 117.62(6) 15 21 ? O3 Na1 O3 62.4(2) 8_655 21 ? O1 Na1 O3 98.97(11) . 12_565 ? O1 Na1 O3 81.03(11) 14_666 12_565 ? F1 Na1 O3 98.97(11) . 12_565 ? F1 Na1 O3 81.03(11) 14_666 12_565 ? O3 Na1 O3 180.0(3) 15 12_565 ? O3 Na1 O3 117.62(6) 8_655 12_565 ? O3 Na1 O3 62.3(2) 21 12_565 ? O1 Na1 O3 81.03(11) . 18 ? O1 Na1 O3 98.97(11) 14_666 18 ? F1 Na1 O3 81.03(11) . 18 ? F1 Na1 O3 98.97(11) 14_666 18 ? O3 Na1 O3 117.62(6) 15 18 ? O3 Na1 O3 180.0(3) 8_655 18 ? O3 Na1 O3 117.62(6) 21 18 ? O3 Na1 O3 62.4(2) 12_565 18 ? O1 Na1 O3 98.97(11) . 4_556 ? O1 Na1 O3 81.03(11) 14_666 4_556 ? F1 Na1 O3 98.97(11) . 4_556 ? F1 Na1 O3 81.03(11) 14_666 4_556 ? O3 Na1 O3 62.4(2) 15 4_556 ? O3 Na1 O3 117.62(6) 8_655 4_556 ? O3 Na1 O3 180.0(3) 21 4_556 ? O3 Na1 O3 117.62(6) 12_565 4_556 ? O3 Na1 O3 62.3(2) 18 4_556 ? O1 Na1 Ta2 90.000(1) . 3_655 ? O1 Na1 Ta2 90.0 14_666 3_655 ? F1 Na1 Ta2 90.000(1) . 3_655 ? F1 Na1 Ta2 90.000(1) 14_666 3_655 ? O3 Na1 Ta2 89.98(12) 15 3_655 ? O3 Na1 Ta2 31.21(12) 8_655 3_655 ? O3 Na1 Ta2 31.21(12) 21 3_655 ? O3 Na1 Ta2 89.98(12) 12_565 3_655 ? O3 Na1 Ta2 148.83(12) 18 3_655 ? O3 Na1 Ta2 148.83(12) 4_556 3_655 ? O1 Na1 Nb2 90.000(1) . 3_655 ? O1 Na1 Nb2 90.0 14_666 3_655 ? F1 Na1 Nb2 90.000(1) . 3_655 ? F1 Na1 Nb2 90.000(1) 14_666 3_655 ? O3 Na1 Nb2 89.98(12) 15 3_655 ? O3 Na1 Nb2 31.21(12) 8_655 3_655 ? O3 Na1 Nb2 31.21(12) 21 3_655 ? O3 Na1 Nb2 89.98(12) 12_565 3_655 ? O3 Na1 Nb2 148.83(12) 18 3_655 ? O3 Na1 Nb2 148.83(12) 4_556 3_655 ? Ta2 Na1 Nb2 0.000(6) 3_655 3_655 ? O1 Na1 H1 0(2) . . ? O1 Na1 H1 180.0(9) 14_666 . ? F1 Na1 H1 0.0(11) . . ? F1 Na1 H1 180.0(6) 14_666 . ? O3 Na1 H1 81.03(11) 15 . ? O3 Na1 H1 98.97(11) 8_655 . ? O3 Na1 H1 81.03(11) 21 . ? O3 Na1 H1 98.97(11) 12_565 . ? O3 Na1 H1 81.03(11) 18 . ? O3 Na1 H1 98.97(11) 4_556 . ? Ta2 Na1 H1 90.000(1) 3_655 . ? Nb2 Na1 H1 90.000(1) 3_655 . ? Nb2 O3 Ta2 0.0 9 9 ? Nb2 O3 Ta1 139.3(3) 9 . ? Ta2 O3 Ta1 139.3(3) 9 . ? Nb2 O3 Na1 103.6(2) 9 4_456 ? Ta2 O3 Na1 103.6(2) 9 4_456 ? Ta1 O3 Na1 104.0(2) . 4_456 ? Nb2 O3 Ca1 104.7(2) 9 3_645 ? Ta2 O3 Ca1 104.7(2) 9 3_645 ? Ta1 O3 Ca1 105.8(2) . 3_645 ? Na1 O3 Ca1 87.52(15) 4_456 3_645 ? Ta2 O2 Nb2 136.7(3) . 9 ? Ta2 O2 Ta2 136.7(3) . 9 ? Nb2 O2 Ta2 0.00(2) 9 9 ? Ta2 O2 Ca1 106.3(2) . . ? Nb2 O2 Ca1 105.2(2) 9 . ? Ta2 O2 Ca1 105.2(2) 9 . ? Ta2 O2 Ca1 105.6(2) . 8_645 ? Nb2 O2 Ca1 103.9(2) 9 8_645 ? Ta2 O2 Ca1 103.9(2) 9 8_645 ? Ca1 O2 Ca1 89.01(15) . 8_645 ? Ca1 F1 Ca1 115.8(9) 5 . ? Ca1 F1 Ca1 115.8(9) 5 9 ? Ca1 F1 Ca1 115.8(9) . 9 ? Ca1 F1 Na1 101.9(14) 5 . ? Ca1 F1 Na1 101.9(14) . . ? Ca1 F1 Na1 101.9(14) 9 . ? Ca1 F1 H1 101.9(14) 5 . ? Ca1 F1 H1 101.9(14) . . ? Ca1 F1 H1 101.9(14) 9 . ? Na1 F1 H1 0.0(16) . . ? Na1 O1 Ca1 112.5(6) . 5 ? Na1 O1 Ca1 112.5(6) . . ? Ca1 O1 Ca1 106.3(6) 5 . ? Na1 O1 Ca1 112.5(6) . 9 ? Ca1 O1 Ca1 106.3(6) 5 9 ? Ca1 O1 Ca1 106.3(6) . 9 ? Na1 O1 H1 0(2) . . ? Ca1 O1 H1 112.5(6) 5 . ? Ca1 O1 H1 112.5(6) . . ? Ca1 O1 H1 112.5(6) 9 . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 33.72 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.281 _refine_diff_density_min -1.369 _refine_diff_density_rms 0.259 loop_ _publcif_info_cif.paper_type ?