In-Depth Study on Chloride Abstractions from (NHC)Ir(COD)Cl Complexes
Sipos, Gellért; Gao, Pengchao; Foster, Daven; Skelton, Brian W.; Sobolev, Alexandre N.; Dorta, Reto; Organometallics 36 (2017) 801–; doi:10.1021/acs.organomet.6b00864

data_4087022
_publ_section_title
;
 In-Depth Study on Chloride Abstractions from (NHC)Ir(COD)Cl Complexes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              801
_journal_paper_doi               10.1021/acs.organomet.6b00864
_journal_volume                  36
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C55 H70 Ir N2, F4 B, C H2 Cl2'
_chemical_formula_sum            'C56 H72 B Cl2 F4 Ir N2'
_chemical_formula_weight         1123.06
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-29T20:54:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.07810(10)
_cell_length_b                   17.6947(2)
_cell_length_c                   25.0413(3)
_cell_measurement_reflns_used    17588
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.234
_cell_measurement_theta_min      2.026
_cell_volume                     4908.69(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX (Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick,G. M., 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, G. M., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.95
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0020669
_diffrn_orient_matrix_UB_12      -0.0244003
_diffrn_orient_matrix_UB_13      0.0224532
_diffrn_orient_matrix_UB_21      -0.033815
_diffrn_orient_matrix_UB_22      -0.02658
_diffrn_orient_matrix_UB_23      -0.0150146
_diffrn_orient_matrix_UB_31      0.0543529
_diffrn_orient_matrix_UB_32      -0.0174674
_diffrn_orient_matrix_UB_33      -0.0084954
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.95
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51554
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        28.5
_diffrn_reflns_theta_max         29.737
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.884
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.52
_exptl_crystal_description       needle
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 4804 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         12922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+2.6739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                12016
_reflns_number_total             12922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00864_si_003.cif
_cod_data_source_block           sg634
_cod_depositor_comments
'Adding full bibliography for 4087022--4087034.cif.'
_cod_database_code               4087022
_shelx_res_checksum              52297
_shelx_hkl_checksum              45242