Expanding the structural versatility of thiostannate(iv) complexes
Nørby, Peter; Eikeland, Espen; Overgaard, Jacob; Johnsen, Simon; Iversen, Bo B.; CrystEngComm 17 (2015) 2413–; doi:10.1039/C4CE02224F

data_7219574
_publ_section_title
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 Expanding the structural versatility of thiostannate(iv) complexes
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2413
_journal_paper_doi               10.1039/C4CE02224F
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'S9 Sn3, 6(H4 N), 4/3(H2 O)'
_chemical_formula_sum            'H26.66667 N6 O1.33333 S9 Sn3'
_chemical_formula_weight         776.88
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-02-11 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0389(9)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   16.98717(13)
_cell_length_b                   10.54777(7)
_cell_length_c                   21.08715(19)
_cell_measurement_reflns_used    32112
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      32.6517
_cell_measurement_theta_min      2.3015
_cell_volume                     3592.61(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0298142000
_diffrn_orient_matrix_UB_12      0.0025238000
_diffrn_orient_matrix_UB_13      -0.0320901000
_diffrn_orient_matrix_UB_21      0.0046933000
_diffrn_orient_matrix_UB_22      -0.0661077000
_diffrn_orient_matrix_UB_23      -0.0038485000
_diffrn_orient_matrix_UB_31      -0.0319004000
_diffrn_orient_matrix_UB_32      -0.0120741000
_diffrn_orient_matrix_UB_33      0.0143651000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            43957
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.726
_diffrn_reflns_theta_min         2.306
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.1599
_exptl_crystal_size_mid          0.1065
_exptl_crystal_size_min          0.0788
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 5368 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         12197
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+1.4488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0338
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.886
_reflns_number_gt                11917
_reflns_number_total             12197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce02224f1.cif
_cod_data_source_block           thiostanante_structure3
_cod_depositor_comments
;
Adding full bibliography for 7219572--7219574.cif.

2019-01-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'H80 N18 O4 S27 Sn9'
_cod_original_formula_weight         2330.65
_cod_original_formula_moiety         '3(S9 Sn3), 18(H4 N), 4(H2 O)'
_cod_original_formula_units_Z            2
_cod_database_code               7219574
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'H20 N4 O1 S6 Sn2'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Others
 Fixed U12: S14(0) Sn4(0) Sn5(0) N3(0) N10(0)
 Fixed U23: S14(0) Sn4(0) Sn5(0) N3(0) N10(0)
 Fixed Uiso: H2E(0.044) H2F(0.044)
 Fixed X: S14(0.5) Sn4(0.5) N3(0.5) N10(0.5) H2E(0.5821) H2F(0.6024)
 Fixed Y: H2E(0.6392) H2F(0.7499)
 Fixed Z: S14(0) Sn4(0) N3(0.5) N10(0.5) H2E(0.1774) H2F(0.2145)
;
_olex2_submission_special_instructions 'No special instructions were received'