Conformational and structural diversity of iridium dimethyl sulfoxide complexes
Ridgway, Benjamin M.; Foi, Ana; Corrêa, Rodrigo S.; Bikiel, Damian E.; Ellena, Javier; Doctorovich, Fabio; Di Salvo, Florencia; Acta Crystallographica Section B 73 (2017) 1032–1042; doi:10.1107/S2052520617011490

data_2108191
_publ_section_title
;
 Conformational and structural diversity of iridium dimethyl sulfoxide
 complexes
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1032
_journal_page_last               1042
_journal_paper_doi               10.1107/S2052520617011490
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         '(C4 H12 Cl4 Ir O2 S2), (C4 H12 N), 0.5H2 O'
_chemical_formula_sum            'C8 H25 Cl4 Ir N O2.5 S2'
_chemical_formula_weight         573.4427
_chemical_name_common
;
'N-Butylammonium tetrachlorobis(dimethyl sulfoxide)iridate(III) hemihydrate'
;
_chemical_name_systematic
;
'N-Butylammonium tetrachlorobis(dimethyl sulfoxide)iridate(III) hemihydrate'
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 108.657(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.8210(4)
_cell_length_b                   10.0830(2)
_cell_length_c                   19.5720(5)
_cell_measurement_reflns_used    32346
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      2.91
_cell_volume                     3706.01(15)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Enraf-Nonius, 1997-2004)'
_computing_data_reduction
;
'DENZO and Scalepack (Otwinowski & Minor 1997)'
;
_computing_molecular_graphics
;
C.B. Hubschle, G.M. Scheldrick, and B. Dittrich
Shelxle: a Qt graphical user interface for SHELXL
J. Appl. Cryst., 44 (2011) 1281--1284
;
_computing_publication_material
;
The PyMol Molecular Graphics System, Version #, Schrodinger, LLC.
Version 1.7.2.1
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18983
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.494
_diffrn_reflns_theta_min         2.926
_exptl_absorpt_coefficient_mu    8.005
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
   P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_description       prism
_exptl_crystal_F_000             2216
_exptl_crystal_recrystallization_method
'Crystallized from DMSO solution of title compound. '
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.530
_refine_diff_density_min         -1.959
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0740P)^2^+31.6594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3050
_reflns_number_total             3424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5014sup1.cif
_cod_data_source_block           1b
_cod_original_formula_sum        'C8 H25 Cl4 Ir1 N1 O2.5 S2'
_cod_database_code               2108191
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.502
_shelx_estimated_absorpt_t_max   0.502
_shelx_res_checksum              24985
_shelx_hkl_checksum              47239
_cod_database_fobs_code 2108191