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_7219572
_publ_section_title
;
 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         '8(C2 H7 N2), S6 Sn2, S4 Sn'
_chemical_formula_sum            'C16 H56 N16 S10 Sn3'
_chemical_formula_weight         1149.43
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4713)
;
_audit_update_record
;
2015-02-11 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.029(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7739(6)
_cell_length_b                   16.0647(3)
_cell_length_c                   11.8936(3)
_cell_measurement_reflns_used    14398
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2715
_cell_measurement_theta_min      2.2077
_cell_volume                     4486.13(18)
_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      100.01(10)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details
;
  1 omega  -63.00   36.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864  -38.0000   60.0000 99

  2 omega  -22.00   85.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864   77.0000    0.0000 107

  3 omega  -46.00   24.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9364   77.0000 -180.0000 70

  4 omega   35.00  101.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864  178.0000   30.0000 66

  5 omega  -16.00   87.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864   38.0000  120.0000 103

  6 omega  -19.00   85.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864   57.0000 -150.0000 104

  7 omega  -20.00   53.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864  -99.0000 -180.0000 73

  8 omega  -19.00   85.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864   57.0000    0.0000 104

  9 omega -100.00  -34.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9364  178.0000  -90.0000 66

 10 omega  -20.00    5.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864  -99.0000   90.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0230454000
_diffrn_orient_matrix_UB_12      -0.0068489000
_diffrn_orient_matrix_UB_13      0.0446401000
_diffrn_orient_matrix_UB_21      0.0188367000
_diffrn_orient_matrix_UB_22      -0.0037294000
_diffrn_orient_matrix_UB_23      -0.0404572000
_diffrn_orient_matrix_UB_31      0.0052384000
_diffrn_orient_matrix_UB_32      0.0434625000
_diffrn_orient_matrix_UB_33      0.0035854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            51708
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.336
_diffrn_reflns_theta_min         2.212
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64267
_exptl_absorpt_correction_type   multi-scan
_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) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_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    1.702
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.439
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+20.3285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4911
_reflns_number_total             6020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce02224f1.cif
_cod_data_source_block           thiostannate_structure1
_cod_depositor_comments
'Adding full bibliography for 7219572--7219574.cif.'
_cod_original_cell_volume        4486.14(19)
_cod_database_code               7219572
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C16H56N16S10Sn3 '
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H12C(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 H5C(0.5) H5D(0.5) H5E(0.5) H2C(0.5) H2D(0.5) H2E(0.5)
 Fixed U12: C11(0) C12(0) C9(0) C10(0) C6(0) C5(0) C2(0) C1(0) S3(0) S4(0)
 S6(0) S7(0) Sn2(0)
 Fixed U23: C11(0) C12(0) C9(0) C10(0) C6(0) C5(0) C2(0) C1(0) S3(0) S4(0)
 S6(0) S7(0) Sn2(0)
 Fixed Uiso: H5A(0.033) H5B(0.033) H1A(0.035) H1B(0.035) H2A(0.028) H2B(0.028)
 H3D(0.025) H3E(0.025)
3.a X=CH2 refined with riding coordinates:
 N7(H7D,H7E), N6(H6A,H6B)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C),
 C5(H5C,H5D,H5E), C2(H2C,H2D,H2E)
;
_olex2_submission_special_instructions 'No special instructions were received'