Surprising discoveries on the way to an old compound: four transient iodido antimonates
Dehnhardt, Natalie; Böth, André; Heine, Johanna; Dalton Transactions  (2019) –; doi:10.1039/C9DT00575G

data_7049395
_publ_section_title
;
 Surprising discoveries on the way to an old compound: four transient
 iodido antimonates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00575G
_journal_year                    2019
_chemical_formula_moiety         '2(I8 Sb2), 2(I3 Sb), 4(C8 H12 Cu N4)'
_chemical_formula_sum            'C32 H48 Cu4 I22 N16 Sb6'
_chemical_formula_weight         4433.32
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a: 2'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-11-26 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.6216(12)
_cell_length_b                   40.6216(12)
_cell_length_c                   12.3875(5)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    110
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.24
_cell_volume                     20440.8(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1436
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            283017
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.332
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.049
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1068 before and 0.0741 after correction. The Ratio of minimum to maximum transmission is 0.6149. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.881
_exptl_crystal_description       prism
_exptl_crystal_F_000             15520
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.897
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         9325
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0229P)^2^+688.6431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6819
_reflns_number_total             9325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00575g2.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        20440.8(15)
_cod_database_code               7049395
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C12(H12A,H12B,
 H12C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              82911
_shelx_fab_checksum              21124
_olex2_submission_special_instructions 'No special instructions were received'