N-Heterocyclic Carbene Functionalized Group 7−9 Transition Metal Phosphinidene Complexes
Aktas, Halil; Slootweg, J. Chris; Ehlers, Andreas W.; Lutz, Martin; Spek, Anthony L.; Lammertsma, Koop; Organometallics 28 (2009) 5166–; doi:10.1021/om900496y

data_4069902
_publ_section_title
;
 N-Heterocyclic Carbene Functionalized Group 7&#x2212;9 Transition Metal
 Phosphinidene Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              5166
_journal_paper_doi               10.1021/om900496y
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C39 H64 N2 P Rh, 0.66(C5 H12)'
_chemical_formula_sum            'C42.3 H71.92 N2 P Rh'
_chemical_formula_weight         742.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 95.432(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4727(3)
_cell_length_b                   15.1067(4)
_cell_length_c                   13.7281(2)
_cell_measurement_reflns_used    18239
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.95
_cell_volume                     2162.14(9)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28979
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             799
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5158
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+1.6907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                4627
_reflns_number_total             5158
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900496y_si_002.cif
_cod_data_source_block           s4069a
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C42.30 H71.92 N2 P Rh'
_cod_database_code               4069902