Interaction of Carbene and Olefin Donors with [Cl2PN]3: Exploration of a Reductive Pathway toward (PN)3
S. M. Ibrahim Al-Rafia; Michael J. Ferguson; Eric Rivard; Inorganic Chemistry 50 (2011) 10543–10545; doi:10.1021/ic201812a

data_4326784
_publ_contact_author_address
;
Department of Chemistry
University of Alberta
Edmonton
AB T6G 2G2
CANADA
;
_publ_contact_author_email       ERIVARD@UALBERTA.CA
_publ_contact_author_name        'E. Rivard'
_publ_section_title
;
 Interaction of Carbene and Olefin Donors with [Cl2PN]3: Exploration of a
 Reductive Pathway toward (PN)3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10543
_journal_page_last               10545
_journal_paper_doi               10.1021/ic201812a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C27 H36 Cl4 N5 P3 S, C7 H8'
_chemical_formula_sum            'C34 H44 Cl4 N5 P3 S'
_chemical_formula_weight         789.51
_chemical_name_common            2
_chemical_name_systematic
; 
 ? 
;
_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                 99.5850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5334(2)
_cell_length_b                   13.9851(2)
_cell_length_c                   24.9658(4)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.28
_cell_measurement_theta_min      3.59
_cell_volume                     3970.66(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Schneider & Sheldrick, 2002)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26061
_diffrn_reflns_theta_full        67.75
_diffrn_reflns_theta_max         69.67
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    4.586
_exptl_absorpt_correction_T_max  0.6160
_exptl_absorpt_correction_T_min  0.3807
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7333
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0683P)^2^+1.6203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1126
_reflns_number_gt                6717
_reflns_number_total             7333
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201812a_si_002_3.cif
_cod_data_source_block           riv1183
_cod_database_code               4326784