Steric and Electronic Influence of Aryl Isocyanides on the Properties of Iridium(III) Cyclometalates.
Maity, Ayan; Le, Linh Q.; Zhu, Zhuan; Bao, Jiming; Teets, Thomas S.; Inorganic chemistry 55 (2016) 2299–2308; doi:10.1021/acs.inorgchem.5b02691

data_4347073
_publ_section_title
;
 Steric and Electronic Influence of Aryl Isocyanides on the Properties of
 Iridium(III) Cyclometalates.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2299
_journal_page_last               2308
_journal_paper_doi               10.1021/acs.inorgchem.5b02691
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C54 H52 Cl6 F6 Ir N4 P S2'
_chemical_formula_weight         1370.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 117.880(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.131(2)
_cell_length_b                   18.910(3)
_cell_length_c                   12.882(2)
_cell_measurement_reflns_used    5442
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.78
_cell_volume                     2827.4(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16315
_diffrn_reflns_point_group_measured_fraction_full 0.686
_diffrn_reflns_point_group_measured_fraction_max 0.595
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.451
_diffrn_reflns_theta_min         1.754
_exptl_absorpt_coefficient_mu    2.807
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
; 
 Classical Flack method preferred over Parsons because s.u. lower. 
;
_refine_ls_abs_structure_Flack   0.000(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         9344
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0344
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.316
_reflns_Friedel_fraction_full    0.377
_reflns_Friedel_fraction_max     0.287
_reflns_number_gt                8063
_reflns_number_total             9344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02691_si_002.cif
_cod_data_source_block           3b
_cod_original_cell_volume        2827.3(9)
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4347073
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              52139
_shelx_hkl_checksum              15975