4-Phosphino-Substituted N-Heterocyclic Carbenes (NHCs) from the Abnormal Reaction of NHCs with Phosphaalkenes
Bates, Joshua I.; Gates, Derek P.; Organometallics 31 (2012) 4529–; doi:10.1021/om3003174

data_4078555
_publ_section_title
;
 4-Phosphino-Substituted N-Heterocyclic Carbenes (NHCs) from the Abnormal
 Reaction of NHCs with Phosphaalkenes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4529
_journal_paper_doi               10.1021/om3003174
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C45 H45 Cl Ir N2 O2 P, C7 H8'
_chemical_formula_sum            'C52 H53 Cl Ir N2 O2 P'
_chemical_formula_weight         996.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.1592(9)
_cell_length_b                   18.3368(6)
_cell_length_c                   17.0683(5)
_cell_measurement_reflns_used    10883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.4
_cell_volume                     9126.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 APEX 2'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            67757
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    3.061
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10883
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+8.8318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0511
_reflns_number_gt                8549
_reflns_number_total             10883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003174_si_001.cif
_cod_data_source_block           dg160_Compound_5Ir
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4078555