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_4326782
_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         'C28 H37 Cl5 N5 P3, C7 H8'
_chemical_formula_sum            'C35 H45 Cl5 N5 P3'
_chemical_formula_weight         805.92
_chemical_name_common            4
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.4845(5)
_cell_angle_beta                 99.7811(5)
_cell_angle_gamma                114.9935(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5636(4)
_cell_length_b                   11.5438(5)
_cell_length_c                   19.1398(8)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.20
_cell_volume                     2030.64(14)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0116
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18102
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.9269
_exptl_absorpt_correction_T_min  0.7380
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         9252
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0662P)^2^+1.2274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                7954
_reflns_number_total             9252
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201812a_si_002_1.cif
_cod_data_source_block           riv1101
_cod_database_code               4326782