Nucleophilicity and P-C Bond Formation Reactions of a Terminal Phosphanido Iridium Complex.
Serrano, Ángel L; Casado, Miguel A.; Ciriano, Miguel A.; de Bruin, Bas; López, José A; Tejel, Cristina; Inorganic chemistry 55 (2016) 828–839; doi:10.1021/acs.inorgchem.5b02301

data_4344585
_publ_section_title
;
 Nucleophilicity and P-C Bond Formation Reactions of a Terminal
 Phosphanido Iridium Complex.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              828
_journal_page_last               839
_journal_paper_doi               10.1021/acs.inorgchem.5b02301
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C23 H24 B Cl Ir N4 O P, 0.4(C6 H6)'
_chemical_formula_sum            'C25.4 H26.4 B Cl Ir N4 O P'
_chemical_formula_weight         673.13
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                110.7038(7)
_cell_angle_beta                 97.3629(7)
_cell_angle_gamma                96.9675(8)
_cell_formula_units_Z            2
_cell_length_a                   9.2577(6)
_cell_length_b                   12.0642(8)
_cell_length_c                   12.3424(8)
_cell_measurement_reflns_used    5052
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.25
_cell_volume                     1258.04(14)
_computing_cell_refinement       'SAINT+ v. 7.66A (Bruker AXS)'
_computing_data_collection       'APEX2 v. 2009-7.0 (Bruker AXS)'
_computing_data_reduction        'SAINT+ v. 7.66A (Bruker AXS)'
_computing_molecular_graphics
;
ORTEP3 for Windows - L. J. Farrugia, 
J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15057
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         1.795
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.503
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2008/1: Area-Detector Absorption Correction. Bruker-AXS 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5470
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0223P)^2^+1.5095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4920
_reflns_number_total             5470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02301_si_002.cif
_cod_data_source_block           ctb87as
_cod_original_cell_volume        1258.03(14)
_cod_original_formula_sum        'C25.40 H26.40 B Cl Ir N4 O P'
_cod_database_code               4344585
_shelx_estimated_absorpt_t_min   0.583
_shelx_estimated_absorpt_t_max   0.810
_shelxl_version_number           2013-4
_shelx_res_checksum              6916
_shelx_hkl_checksum              9638