Syntheses, Structures, and Reactivity of Barium Carbene Complexes with Chelating Bis-iminophosphorano Arms
Orzechowski, Lars; Harder, Sjoerd; Organometallics 26 (2007) 5501–; doi:10.1021/om700640c

data_4073808
_publ_section_title
;
 Syntheses, Structures, and Reactivity of Barium Carbene Complexes with
 Chelating Bis-iminophosphorano Arms
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5501
_journal_paper_doi               10.1021/om700640c
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C134 H156 Ba2 N6 O3 P4'
_chemical_formula_weight         2297.20
_chemical_name_common            {Ba[CyNC(O)C(Ph2P=N-DIPP)2]}2.THF
_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                89.555(3)
_cell_angle_beta                 79.116(3)
_cell_angle_gamma                64.692(3)
_cell_formula_units_Z            2
_cell_length_a                   15.2106(8)
_cell_length_b                   17.7038(9)
_cell_length_c                   24.3033(12)
_cell_measurement_temperature    203(2)
_cell_volume                     5790.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            90240
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    0.787
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2396
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         26243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+1.7724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                20171
_reflns_number_total             26243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700640c-file004.cif
_cod_data_source_block           hasj72
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C67 H78 Ba N3 O1.50 P2'
_cod_database_code               4073808