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_7049392
_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
'I8 Sb2, I5 Sb, 4(I3 Sb), 4(C8 H12 Cu N4), C2 H3 N'
_chemical_formula_sum            'C34 H51 Cu4 I25 N17 Sb7'
_chemical_formula_weight         4976.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-26 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.644(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4510(6)
_cell_length_b                   39.343(2)
_cell_length_c                   13.3623(7)
_cell_measurement_reflns_used    9153
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.06
_cell_measurement_theta_min      2.28
_cell_volume                     5264.0(5)
_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      99.99
_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  0.1369
_diffrn_reflns_av_unetI/netI     0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            109253
_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         25.312
_diffrn_reflns_theta_min         2.194
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.919
_exptl_absorpt_correction_T_max  0.1479
_exptl_absorpt_correction_T_min  0.1033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1286 before and 0.0761 after correction.
The Ratio of minimum to maximum transmission is 0.6984.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.140
_exptl_crystal_description       plate
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.055
_refine_diff_density_max         3.269
_refine_diff_density_min         -1.807
_refine_diff_density_rms         0.373
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         19152
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0674
_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^)+(0.0394P)^2^+134.6056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                14133
_reflns_number_total             19152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00575g2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        5264.1(5)
_cod_database_code               7049392
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.375
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.61(8)
 0.39(8)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C31) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(N6) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(N7) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N14)
\\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N16) \\sim Ueq,
Uanis(N13) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C2(H2A,H2B,
 H2C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C18(H18A,H18B,
 H18C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C26(H26A,H26B,H26C), C32(H32A,H32B,
 H32C), C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C16(H16A,H16B,H16C), C10(H10A,
 H10B,H10C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              47067
_olex2_submission_special_instructions 'No special instructions were received'