Synthesis and Coordination Chemistry of a Tridentateo-Phenylene-Bridged Diphosphine−NHC System
Steinke, Tobias; Shaw, Bryan K.; Jong, Howard; Patrick, Brian O.; Fryzuk, Michael D.; Organometallics 28 (2009) 2830–; doi:10.1021/om9000764

data_4069219
_publ_section_title
;
 Synthesis and Coordination Chemistry of a Tridentateo-Phenylene-Bridged
 Diphosphine&#x2212;NHC System
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2830
_journal_paper_doi               10.1021/om9000764
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C27 H41 F6 N2 P3'
_chemical_formula_weight         600.53
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 109.652(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.9249(11)
_cell_length_b                   10.6491(4)
_cell_length_c                   20.8683(8)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.3946
_cell_measurement_theta_min      2.3995
_cell_volume                     6262.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37854
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         26.80
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_correction_T_min  0.7931
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.00000(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6678
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          1.834
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+13.4922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1958
_reflns_number_gt                4934
_reflns_number_total             6678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9000764_si_002.cif
_cod_data_source_block           mf672
_cod_database_code               4069219