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_7049394
_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         'I4 Sb, I3 Sb, C8 H12 Cu N4'
_chemical_formula_sum            'C8 H12 Cu I7 N4 Sb2'
_chemical_formula_weight         1359.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-26 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.449(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3965(2)
_cell_length_b                   16.7953(7)
_cell_length_c                   21.6770(7)
_cell_measurement_reflns_used    26975
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.24
_cell_measurement_theta_min      1.88
_cell_volume                     2690.40(16)
_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      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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  0.1101
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            55242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.980
_diffrn_reflns_theta_min         1.881
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.810
_exptl_absorpt_correction_T_max  0.5577
_exptl_absorpt_correction_T_min  0.2349
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-Red32 1.63.4'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.357
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.675
_refine_diff_density_min         -3.415
_refine_diff_density_rms         0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.805
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         9237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.805
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6076
_reflns_number_total             9237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00575g2.cif
_cod_data_source_block           compound4
_cod_database_code               7049394
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.568
_shelx_estimated_absorpt_t_min   0.179
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              4996
_olex2_submission_special_instructions 'No special instructions were received'