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_4327577
_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
'((C5 H4 N) C (P(C6 H5)2)2)((C5 H4 N C H (P(C6 H5)2)2) Ir H (B F4) (C4 H10 O)'
_chemical_formula_sum            'C64 H60 B F4 Ir N2 O P4'
_chemical_formula_weight         1276.03
_chemical_name_systematic
; 
 Hydrido(\h^2^-(2-pyridylbis(diphenylphosphino)methanido)(\h^3^-2-pyridyl 
 bis(diphenylphosphino)methane)iridium(III) tetrafluoroborate diethyl ether 
 solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.081(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1837(10)
_cell_length_b                   21.329(2)
_cell_length_c                   18.365(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.778
_cell_measurement_theta_min      17.609
_cell_volume                     5873.0(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10843
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        5.3
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.438
_exptl_absorpt_correction_T_max  0.2713
_exptl_absorpt_correction_T_min  0.2201
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scans (North, et al., 1968)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       Block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         10423
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+1.4392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                6935
_reflns_number_total             10423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0012662B_11.cif
_cod_data_source_block           15
_cod_database_code               4327577