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_7049393
_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         '3(I7 Sb2), I4 Sb, 3(I3 Sb), 4(C8 H12 Cu N4)'
_chemical_formula_sum            'C32 H48 Cu4 I34 N16 Sb10'
_chemical_formula_weight         6443.12
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-11-26 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                107.700(3)
_cell_angle_beta                 94.743(3)
_cell_angle_gamma                93.000(3)
_cell_formula_units_Z            1
_cell_length_a                   12.8463(4)
_cell_length_b                   13.0686(4)
_cell_length_c                   19.1151(6)
_cell_measurement_reflns_used    39114
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      1.60
_cell_volume                     3036.56(17)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       'area detetor, \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            30447
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.198
_diffrn_reflns_theta_min         1.596
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.541
_exptl_absorpt_correction_T_max  0.2641
_exptl_absorpt_correction_T_min  0.1401
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE XRED32 1.53'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.523
_exptl_crystal_description       block
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.173
_refine_diff_density_max         1.682
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.232
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(5)
_refine_ls_extinction_coef       0.000259(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.796
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         30447
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.796
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                19544
_reflns_number_total             30447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00575g2.cif
_cod_data_source_block           compound3
_cod_database_code               7049393
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.77(5)
 0.23(5)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C13-C14
 1.2 with sigma of 0.02
 C25-C26
 1.2 with sigma of 0.02
 N5-C10
 -2.5 with sigma of 0.02
 C14-C13
 -1.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C14) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C20(H20A,H20B,
 H20C), C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C8(H8A,H8B,H8C), C4(H4A,
 H4B,H4C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C),
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              392
_olex2_submission_special_instructions 'No special instructions were received'