Template Synthesis of Donor-Functionalized NX-Carbenes (X = P, Si)
Yu, Insun; Wallis, Christopher J.; Patrick, Brian O.; Mehrkhodavandi, Parisa; Organometallics 28 (2009) 6370–; doi:10.1021/om900725e

data_4070333
_publ_section_title
;
 Template Synthesis of Donor-Functionalized NX-Carbenes (X = P, Si)
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6370
_journal_paper_doi               10.1021/om900725e
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C40 H36 Fe N O P Si'
_chemical_formula_weight         661.61
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   20.407(3)
_cell_length_b                   10.1257(12)
_cell_length_c                   15.793(2)
_cell_measurement_reflns_used    4531
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.47
_cell_measurement_theta_min      2.38
_cell_volume                     3263.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21711
_diffrn_reflns_theta_full        23.73
_diffrn_reflns_theta_max         23.73
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                4208
_reflns_number_total             4952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900725e_si_001.cif
_cod_data_source_block           pm039
_cod_original_cell_volume        3263.3(7)
_cod_original_sg_symbol_H-M      'P na21'
_cod_database_code               4070333