Structural diversity in copper(I) iodide complexes with 6-thioxopiperidin-2-one, piperidine-2,6-dithione and isoindoline-1,3-dithione ligands
Wheaton, Amelia M.; Guzei, Ilia A.; Berry, John F.; Acta Crystallographica Section E 76 (2020) 1336–1344; doi:10.1107/S2056989020009676

data_2243503
_publ_section_title
;
 Structural diversity in copper(I) iodide complexes with
 6-thioxopiperidin-2-one, piperidine-2,6-dithione and
 isoindoline-1,3-dithione ligands
;
_journal_coeditor_code           ZL2791
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1336
_journal_page_last               1344
_journal_paper_doi               10.1107/S2056989020009676
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Cu4 I4 (C2 H3 N)2 (C5 H7 N O S)2]'
_chemical_formula_moiety         'C14 H20 Cu4 I4 N4 O2 S2'
_chemical_formula_sum            'C14 H20 Cu4 I4 N4 O2 S2'
_chemical_formula_weight         1102.22
_chemical_name_systematic
Bis(acetonitrile-\k<i>N</i>)tetra-\m~3~-iodido-bis(6-sulfanylidenepiperidin-2-one-\k<i>S</i>)-<i>tetrahedro</i>-tetracopper(I)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
OLEX2
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.562(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4669(8)
_cell_length_b                   12.2157(7)
_cell_length_c                   16.9969(11)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    104.97
_cell_measurement_theta_max      73.443
_cell_measurement_theta_min      4.905
_cell_volume                     2773.9(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      104.97
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEXII area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23553
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.436
_diffrn_reflns_theta_min         4.905
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           32.0
_diffrn_source_power             1.28
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    39.972
_exptl_absorpt_correction_T_max  0.1882
_exptl_absorpt_correction_T_min  0.0419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.837
_refine_diff_density_min         -1.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2753
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0336P)^2^+8.1228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                2669
_reflns_number_total             2753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2791sup1.cif
_cod_data_source_block           II
_cod_database_code               2243503
_shelx_estimated_absorpt_t_min   0.108
_shelx_estimated_absorpt_t_max   0.298
_shelx_hkl_checksum              58559
_shelx_res_checksum              54140
_cod_database_fobs_code 2243503