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_4078551
_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         'C43 H45 N2 P, 0.5(C6 H6)'
_chemical_formula_sum            'C46 H48 N2 P'
_chemical_formula_weight         659.83
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 117.843(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.5920(15)
_cell_length_b                   15.3880(9)
_cell_length_c                   18.6930(11)
_cell_measurement_reflns_used    9259
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.2
_cell_volume                     7781.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43060
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+3.8196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                5627
_reflns_number_total             9259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003174_si_001.cif
_cod_data_source_block           dg113_0m_Compound_1a
_cod_original_cell_volume        7781.0(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4078551