Iminophosphide Bonding Environments from Carbene Complexes of Iminophosphines
Neil Burford; T. Stanley Cameron; Daren J. LeBlanc; Andrew D. Phillips; Thomas E. Concolino; Kin-Chung Lam; Arnold L. Rheingold; Journal of the American Chemical Society 122 (2000) 5413–5414; doi:10.1021/ja000432+

data_4116021
_publ_contact_author_address
;  Department of Chemistry
   Dalhousie University
   Halifax, NS B3H 4J3
   CANADA
;
_publ_contact_author_email       burford@chem1.chem.dal.ca
_publ_contact_author_fax         '(902) 494-1310'
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       '(902) 494-3190'
_publ_section_title
;
 Iminophosphide Bonding Environments from Carbene Complexes of
 Iminophosphines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5413
_journal_page_last               5414
_journal_paper_doi               10.1021/ja000432+
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C29 H49 Cl N3 P'
_chemical_formula_weight         506.13
_chemical_temperature_decomposition 450(1)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.8920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8062(3)
_cell_length_b                   8.51840(10)
_cell_length_c                   17.8511(2)
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3097.91(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9422
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.9438
_exptl_absorpt_correction_T_min  0.9260
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1374P)^2^+12.8850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2371
_refine_ls_wR_factor_ref         0.2753
_reflns_number_gt                3497
_reflns_number_total             4217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0004322B_2.cif
_cod_data_source_block           burla_7a
_cod_original_cell_volume        3097.90(7)
_cod_database_code               4116021