#------------------------------------------------------------------------------
#$Date: 2016-10-14 08:18:43 +0200 (vie 14 de oct de 2016) $
#$Revision: 187333 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/67/7226798.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7226798
loop_
_publ_author_name
'Wu, Xiaowen'
'Hu, Yi'
'Pan, Hui'
'Su, Zhi'
_publ_section_title
;
 Na9Sb(Ge2Q6)2 (Q = S, Se): two new antimony (III) quaternary
 chalcogenides with ethane-like [Ge2Q6]6− ligands
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA22000B
_journal_year                    2016
_chemical_formula_sum            'Ge4 Na9 S12 Sb'
_chemical_formula_weight         1003.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-06-06 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.587(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   7.5857(7)
_cell_length_b                   11.5743(11)
_cell_length_c                   6.8175(11)
_cell_measurement_reflns_used    1898
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      3.12
_cell_volume                     573.66(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3251
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    7.595
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0216P)²+0.8587P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                474
_reflns_number_total             512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra22000b1.cif
_cod_data_source_block           666
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      'C2/m  '
_cod_database_code               7226798
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
Ge1 Ge 0.16461(6) 0.5000 0.55624(6) 0.01248(16) Uani 1 2 d S
Sb1 Sb 0.0000 0.18408(7) 0.5000 0.0195(2) Uani 0.25 2 d SP
Na1 Na 0.0000 0.18408(7) 0.5000 0.0195(2) Uani 0.75 2 d SP
S1 S 0.25302(11) 0.34189(7) 0.74327(10) 0.0244(2) Uani 1 1 d .
S2 S 0.26546(16) 0.5000 0.28352(15) 0.0254(3) Uani 1 2 d S
Na2 Na 0.5000 0.5000 0.0000 0.0291(6) Uani 1 4 d S
Na3 Na 0.0000 0.34159(17) 0.0000 0.0321(5) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
S2 Ge1 S1 111.32(3) . 6_565
S2 Ge1 S1 111.32(3) . .
S1 Ge1 S1 110.91(4) 6_565 .
S2 Ge1 Ge1 108.15(4) . 5_566
S1 Ge1 Ge1 107.47(3) 6_565 5_566
S1 Ge1 Ge1 107.47(3) . 5_566
S2 Ge1 Na2 113.88(4) . 1_556
S1 Ge1 Na2 56.97(2) 6_565 1_556
S1 Ge1 Na2 56.97(2) . 1_556
Ge1 Ge1 Na2 137.98(3) 5_566 1_556
S2 Ge1 Na1 57.13(2) . 3
S1 Ge1 Na1 55.90(3) 6_565 3
S1 Ge1 Na1 117.69(3) . 3
Ge1 Ge1 Na1 134.819(14) 5_566 3
Na2 Ge1 Na1 72.789(10) 1_556 3
S2 Ge1 Na1 57.13(2) . 7_556
S1 Ge1 Na1 117.69(3) 6_565 7_556
S1 Ge1 Na1 55.90(3) . 7_556
Ge1 Ge1 Na1 134.819(14) 5_566 7_556
Na2 Ge1 Na1 72.789(10) 1_556 7_556
Na1 Ge1 Na1 76.99(2) 3 7_556
S1 Sb1 S1 99.27(4) . 2_556
S1 Sb1 S1 100.15(3) . 8_455
S1 Sb1 S1 87.73(3) 2_556 8_455
S1 Sb1 S1 87.73(3) . 7_556
S1 Sb1 S1 100.15(3) 2_556 7_556
S1 Sb1 S1 167.90(5) 8_455 7_556
S1 Sb1 S2 172.90(3) . 3_445
S1 Sb1 S2 87.75(2) 2_556 3_445
S1 Sb1 S2 78.97(3) 8_455 3_445
S1 Sb1 S2 92.07(3) 7_556 3_445
S1 Sb1 S2 87.75(2) . 7_556
S1 Sb1 S2 172.90(3) 2_556 7_556
S1 Sb1 S2 92.07(3) 8_455 7_556
S1 Sb1 S2 78.97(3) 7_556 7_556
S2 Sb1 S2 85.24(4) 3_445 7_556
Ge1 S1 Sb1 98.78(3) . .
Ge1 S1 Na2 81.99(3) . 1_556
Sb1 S1 Na2 177.72(3) . 1_556
Ge1 S1 Sb1 83.90(3) . 7_556
Sb1 S1 Sb1 92.27(3) . 7_556
Na2 S1 Sb1 89.94(3) 1_556 7_556
Ge1 S1 Na1 83.90(3) . 7_556
Sb1 S1 Na1 92.27(3) . 7_556
Na2 S1 Na1 89.94(3) 1_556 7_556
Sb1 S1 Na1 0.00(3) 7_556 7_556
Ge1 S1 Na3 101.59(5) . 1_556
Sb1 S1 Na3 84.21(3) . 1_556
Na2 S1 Na3 93.54(3) 1_556 1_556
Sb1 S1 Na3 173.85(5) 7_556 1_556
Na1 S1 Na3 173.85(5) 7_556 1_556
Ge1 S1 Na3 160.53(4) . 7_556
Sb1 S1 Na3 95.19(4) . 7_556
Na2 S1 Na3 84.57(3) 1_556 7_556
Sb1 S1 Na3 82.05(3) 7_556 7_556
Na1 S1 Na3 82.05(3) 7_556 7_556
Na3 S1 Na3 93.22(3) 1_556 7_556
Ge1 S2 Na1 83.15(3) . 3
Ge1 S2 Sb1 83.15(3) . 3
Na1 S2 Sb1 0.00(2) 3 3
Ge1 S2 Na1 83.15(3) . 7_556
Na1 S2 Na1 94.76(4) 3 7_556
Sb1 S2 Na1 94.76(4) 3 7_556
Ge1 S2 Sb1 83.15(3) . 7_556
Na1 S2 Sb1 94.76(4) 3 7_556
Sb1 S2 Sb1 94.76(4) 3 7_556
Na1 S2 Sb1 0.00(2) 7_556 7_556
Ge1 S2 Na2 164.50(5) . .
Na1 S2 Na2 86.38(3) 3 .
Sb1 S2 Na2 86.38(3) 3 .
Na1 S2 Na2 86.38(3) 7_556 .
Sb1 S2 Na2 86.38(3) 7_556 .
Ge1 S2 Na3 102.33(4) . .
Na1 S2 Na3 169.64(4) 3 .
Sb1 S2 Na3 169.64(4) 3 .
Na1 S2 Na3 94.63(3) 7_556 .
Sb1 S2 Na3 94.63(3) 7_556 .
Na2 S2 Na3 89.85(3) . .
Ge1 S2 Na3 102.33(4) . 5_565
Na1 S2 Na3 94.63(3) 3 5_565
Sb1 S2 Na3 94.63(3) 3 5_565
Na1 S2 Na3 169.64(4) 7_556 5_565
Sb1 S2 Na3 169.64(4) 7_556 5_565
Na2 S2 Na3 89.85(3) . 5_565
Na3 S2 Na3 75.69(6) . 5_565
S1 Na2 S1 180.0 1_554 5_666
S1 Na2 S1 99.67(3) 1_554 2_656
S1 Na2 S1 80.33(3) 5_666 2_656
S1 Na2 S1 80.33(3) 1_554 6_564
S1 Na2 S1 99.67(3) 5_666 6_564
S1 Na2 S1 180.0 2_656 6_564
S1 Na2 S2 89.36(2) 1_554 .
S1 Na2 S2 90.64(2) 5_666 .
S1 Na2 S2 90.64(2) 2_656 .
S1 Na2 S2 89.36(2) 6_564 .
S1 Na2 S2 90.64(2) 1_554 5_665
S1 Na2 S2 89.36(2) 5_666 5_665
S1 Na2 S2 89.36(2) 2_656 5_665
S1 Na2 S2 90.64(2) 6_564 5_665
S2 Na2 S2 180.0 . 5_665
S1 Na2 Ge1 138.965(15) 1_554 5_666
S1 Na2 Ge1 41.035(15) 5_666 5_666
S1 Na2 Ge1 41.035(15) 2_656 5_666
S1 Na2 Ge1 138.965(15) 6_564 5_666
S2 Na2 Ge1 81.62(2) . 5_666
S2 Na2 Ge1 98.38(2) 5_665 5_666
S1 Na2 Ge1 41.035(15) 1_554 1_554
S1 Na2 Ge1 138.965(15) 5_666 1_554
S1 Na2 Ge1 138.965(15) 2_656 1_554
S1 Na2 Ge1 41.035(15) 6_564 1_554
S2 Na2 Ge1 98.38(2) . 1_554
S2 Na2 Ge1 81.62(2) 5_665 1_554
Ge1 Na2 Ge1 180.0 5_666 1_554
S1 Na2 Na3 49.834(16) 1_554 7
S1 Na2 Na3 130.166(16) 5_666 7
S1 Na2 Na3 49.834(16) 2_656 7
S1 Na2 Na3 130.166(16) 6_564 7
S2 Na2 Na3 90.0 . 7
S2 Na2 Na3 90.0 5_665 7
Ge1 Na2 Na3 90.0 5_666 7
Ge1 Na2 Na3 90.0 1_554 7
S1 Na2 Na3 130.166(16) 1_554 3
S1 Na2 Na3 49.834(16) 5_666 3
S1 Na2 Na3 130.166(16) 2_656 3
S1 Na2 Na3 49.834(16) 6_564 3
S2 Na2 Na3 90.0 . 3
S2 Na2 Na3 90.0 5_665 3
Ge1 Na2 Na3 90.0 5_666 3
Ge1 Na2 Na3 90.0 1_554 3
Na3 Na2 Na3 180.0 7 3
S1 Na2 Na1 45.161(18) 1_554 7
S1 Na2 Na1 134.839(18) 5_666 7
S1 Na2 Na1 91.226(19) 2_656 7
S1 Na2 Na1 88.774(19) 6_564 7
S2 Na2 Na1 134.040(16) . 7
S2 Na2 Na1 45.960(16) 5_665 7
Ge1 Na2 Na1 125.573(10) 5_666 7
Ge1 Na2 Na1 54.427(10) 1_554 7
Na3 Na2 Na1 57.993(10) 7 7
Na3 Na2 Na1 122.007(10) 3 7
S1 Na2 Na1 134.839(18) 1_554 3
S1 Na2 Na1 45.161(18) 5_666 3
S1 Na2 Na1 88.774(19) 2_656 3
S1 Na2 Na1 91.226(19) 6_564 3
S2 Na2 Na1 45.960(16) . 3
S2 Na2 Na1 134.040(16) 5_665 3
Ge1 Na2 Na1 54.427(10) 5_666 3
Ge1 Na2 Na1 125.573(10) 1_554 3
Na3 Na2 Na1 122.007(10) 7 3
Na3 Na2 Na1 57.993(10) 3 3
Na1 Na2 Na1 180.000(18) 7 3
S1 Na3 S1 179.87(8) 2_556 1_554
S1 Na3 S2 92.76(4) 2_556 .
S1 Na3 S2 87.16(4) 1_554 .
S1 Na3 S2 87.16(4) 2_556 5_565
S1 Na3 S2 92.76(4) 1_554 5_565
S2 Na3 S2 104.31(6) . 5_565
S1 Na3 S1 86.78(3) 2_556 8_454
S1 Na3 S1 93.32(4) 1_554 8_454
S2 Na3 S1 173.39(6) . 8_454
S2 Na3 S1 82.26(2) 5_565 8_454
S1 Na3 S1 93.32(4) 2_556 7_556
S1 Na3 S1 86.78(3) 1_554 7_556
S2 Na3 S1 82.26(2) . 7_556
S2 Na3 S1 173.39(6) 5_565 7_556
S1 Na3 S1 91.19(6) 8_454 7_556
S1 Na3 Na3 89.93(4) 2_556 5_565
S1 Na3 Na3 89.93(4) 1_554 5_565
S2 Na3 Na3 52.15(3) . 5_565
S2 Na3 Na3 52.15(3) 5_565 5_565
S1 Na3 Na3 134.40(3) 8_454 5_565
S1 Na3 Na3 134.40(3) 7_556 5_565
S1 Na3 Na1 133.55(4) 2_556 1_554
S1 Na3 Na1 46.54(2) 1_554 1_554
S2 Na3 Na1 133.64(2) . 1_554
S2 Na3 Na1 83.61(2) 5_565 1_554
S1 Na3 Na1 46.91(2) 8_454 1_554
S1 Na3 Na1 91.33(4) 7_556 1_554
Na3 Na3 Na1 118.14(3) 5_565 1_554
S1 Na3 Na2 90.07(4) 2_556 3_445
S1 Na3 Na2 90.07(4) 1_554 3_445
S2 Na3 Na2 127.85(3) . 3_445
S2 Na3 Na2 127.85(3) 5_565 3_445
S1 Na3 Na2 45.60(3) 8_454 3_445
S1 Na3 Na2 45.60(3) 7_556 3_445
Na3 Na3 Na2 180.0 5_565 3_445
Na1 Na3 Na2 61.86(3) 1_554 3_445
S1 Na3 Na2 42.24(2) 2_556 1_455
S1 Na3 Na2 137.68(4) 1_554 1_455
S2 Na3 Na2 99.99(4) . 1_455
S2 Na3 Na2 44.97(2) 5_565 1_455
S1 Na3 Na2 84.087(17) 8_454 1_455
S1 Na3 Na2 135.40(2) 7_556 1_455
Na3 Na3 Na2 64.20(2) 5_565 1_455
Na1 Na3 Na2 115.588(4) 1_554 1_455
Na2 Na3 Na2 115.80(2) 3_445 1_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 S2 2.2033(12) .
Ge1 S1 2.2218(8) 6_565
Ge1 S1 2.2218(8) .
Ge1 Ge1 2.3940(8) 5_566
Ge1 Na2 3.3512(5) 1_556
Ge1 Na1 3.4229(6) 3
Ge1 Na1 3.4229(6) 7_556
Sb1 S1 2.8202(9) .
Sb1 S1 2.8202(9) 2_556
Sb1 S1 2.8504(9) 8_455
Sb1 S1 2.8504(9) 7_556
Sb1 S2 2.8954(9) 3_445
Sb1 S2 2.8954(9) 7_556
S1 Na2 2.8373(8) 1_556
S1 Sb1 2.8504(9) 7_556
S1 Na1 2.8504(9) 7_556
S1 Na3 2.9437(9) 1_556
S1 Na3 3.0349(16) 7_556
S2 Na1 2.8954(9) 3
S2 Sb1 2.8954(9) 3
S2 Na1 2.8954(9) 7_556
S2 Sb1 2.8954(9) 7_556
S2 Na2 2.9774(12) .
S2 Na3 2.9884(15) .
S2 Na3 2.9884(15) 5_565
Na2 S1 2.8373(8) 1_554
Na2 S1 2.8373(8) 5_666
Na2 S1 2.8373(8) 2_656
Na2 S1 2.8373(8) 6_564
Na2 S2 2.9774(12) 5_665
Na2 Ge1 3.3512(5) 5_666
Na2 Ge1 3.3513(5) 1_554
Na2 Na3 3.954(2) 7
Na2 Na3 3.954(2) 3
Na2 Na1 4.0198(6) 7
Na2 Na1 4.0198(6) 3
Na3 S1 2.9437(9) 2_556
Na3 S1 2.9437(9) 1_554
Na3 S2 2.9884(15) 5_565
Na3 S1 3.0349(16) 8_454
Na3 S1 3.0349(16) 7_556
Na3 Na3 3.667(4) 5_565
Na3 Na1 3.8657(11) 1_554
Na3 Na2 3.954(2) 3_445
Na3 Na2 4.2128(9) 1_455
