Synthetic and Structural Studies of the Coordination Behavior of 2-Pyridylbis(diphenylphosphino)methane
Joel T. Mague; Jamin L. Krinsky; Inorganic Chemistry 40 (2001) 1962–1971; doi:10.1021/ic001266+

data_4327570
_publ_section_title
;
 Synthetic and Structural Studies of the Coordination Behavior of
 2-Pyridylbis(diphenylphosphino)methane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1962
_journal_page_last               1971
_journal_paper_doi               10.1021/ic001266+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
'(C O)3 Br (((C6 H5)2 P)2 C H (C5 H4 N) Re (C3 H6 O)0.75'
_chemical_formula_sum            'C35.25 H29.5 Br N O3.75 P2 Re'
_chemical_formula_weight         855.15
_chemical_name_systematic
; 
 fac-Bromo(2-pyridylbis(diphenylphosphino)methane)tricarbonylrhenium(I) 
 acetone solvate
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.175(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0065(19)
_cell_length_b                   10.8139(7)
_cell_length_c                   20.6781(18)
_cell_measurement_reflns_used    2
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.16
_cell_measurement_theta_min      16.15
_cell_volume                     3469.3(6)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1987)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1997)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\q/2\q 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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.1196
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6347
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        10
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.783
_exptl_absorpt_correction_T_max  0.7139
_exptl_absorpt_correction_T_min  0.3776
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scan (North et al., 1968)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       Block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.880
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6128
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                3605
_reflns_number_total             6128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0012662B_04.cif
_cod_data_source_block           4
_cod_original_cell_volume        3469.3(5)
_cod_original_formula_sum        'C35.25 H29.50 Br N O3.75 P2 Re'
_cod_database_code               4327570