Synthesis, Structures, and Reactions of Dirhodium Complexes Bearing a 1,2-Diphenyl-3,4-diphosphinidenecyclobutene Ligand (DPCB)
Okazaki, Masaaki; Hayashi, Akito; Fu, Ching-Feng; Liu, Shiuh-Tzung; Ozawa, Fumiyuki; Organometallics 28 (2009) 902–; doi:10.1021/om8010799

data_4068766
_publ_section_title
;
 Synthesis, Structures, and Reactions of Dirhodium Complexes Bearing a
 1,2-Diphenyl-3,4-diphosphinidenecyclobutene Ligand (DPCB)
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              902
_journal_paper_doi               10.1021/om8010799
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration unk
_chemical_formula_sum            'C105 H140 O P4 Rh2'
_chemical_formula_weight         1747.87
_chemical_properties_physical    air-sensitive
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                71.572(11)
_cell_angle_beta                 68.830(9)
_cell_angle_gamma                68.024(10)
_cell_formula_units_Z            2
_cell_length_a                   15.1401(15)
_cell_length_b                   19.3117(19)
_cell_length_c                   20.181(2)
_cell_measurement_reflns_used    11930
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0043
_cell_volume                     4989.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40137
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.9411
_exptl_absorpt_correction_T_min  0.8796
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Higashi
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.321
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1050
_refine_ls_number_reflns         21779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+6.3987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                17792
_reflns_number_total             21779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010799_si_001.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        4989.7(9)
_cod_database_code               4068766