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_4344584
_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         'C35 H34 B Ir N4 O P2, 0.5(C6 H14)'
_chemical_formula_sum            'C38 H41 B Ir N4 O P2'
_chemical_formula_weight         834.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.314(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2199(6)
_cell_length_b                   16.3663(11)
_cell_length_c                   23.4311(16)
_cell_measurement_reflns_used    5619
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.46
_cell_volume                     3520.5(4)
_computing_cell_refinement       'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 4.0 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_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    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31297
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.520
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.920
_exptl_absorpt_correction_T_max  0.7720
_exptl_absorpt_correction_T_min  0.5858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2008/1: Area-Detector Absorption Correction. Bruker-AXS 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       plate
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7682
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0295P)^2^+2.5230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5522
_reflns_number_total             7682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02301_si_002.cif
_cod_data_source_block           ctb96as
_cod_database_code               4344584
_shelx_estimated_absorpt_t_min   0.488
_shelx_estimated_absorpt_t_max   0.929
_shelxl_version_number           2013-4
_shelx_res_checksum              56209
_shelx_hkl_checksum              19599