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_4078554
_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         '2(C51 H57 Cl Ir N2 P), 3(C H2 Cl2)'
_chemical_formula_sum            'C105 H120 Cl8 Ir2 N4 P2'
_chemical_formula_weight         2167.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.941(4)
_cell_angle_beta                 68.341(5)
_cell_angle_gamma                76.550(4)
_cell_formula_units_Z            2
_cell_length_a                   15.9409(13)
_cell_length_b                   16.1210(12)
_cell_length_c                   20.8548(15)
_cell_measurement_reflns_used    36890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      1.3
_cell_volume                     4823.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            116130
_diffrn_reflns_theta_full        28.18
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    3.061
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'twinabs 2008/2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .1
_refine_diff_density_max         3.082
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         36890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+45.6204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                30190
_reflns_number_total             36890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003174_si_001.cif
_cod_data_source_block           dg155t_Compound_4Ir
_cod_original_cell_volume        4823.0(6)
_cod_database_code               4078554