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_2243506
_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_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_absolute_configuration ad
_chemical_formula_iupac          '[Cu I (C8 H5 N S2)]'
_chemical_formula_moiety         'C8 H5 Cu I N S2'
_chemical_formula_sum            'C8 H5 Cu I N S2'
_chemical_formula_weight         369.69
_chemical_name_systematic
Poly[(\m-isoindoline-1,3-dithione-\k^2^<i>S</i>:<i>S</i>)copper(I)]-\m~3~-iodido]
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_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                 92.98(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.174(5)
_cell_length_b                   4.1188(16)
_cell_length_c                   15.785(6)
_cell_measurement_reflns_used    4507
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.885
_cell_measurement_theta_min      2.584
_cell_volume                     985.2(6)
_computing_cell_refinement
;
APEX3  (Bruker, 2017)
;
_computing_data_collection
;
APEX3  (Bruker, 2017)
;
_computing_data_reduction
;
APEX3  (Bruker, 2017)
;
_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      100.0
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11871
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         33.190
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.720
_exptl_absorpt_correction_T_max  0.4036
_exptl_absorpt_correction_T_min  0.3220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.016
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.174
_refine_diff_density_min         -1.131
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1438 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.034(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         3603
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0417P)^2^+7.0163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                3226
_reflns_number_total             3603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2791sup1.cif
_cod_data_source_block           V
_cod_database_code               2243506
_shelx_estimated_absorpt_t_min   0.281
_shelx_estimated_absorpt_t_max   0.945
_shelx_hkl_checksum              7467
_shelx_res_checksum              44794
_cod_database_fobs_code 2243506