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_4068764
_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_moiety         'C114 H162 O2 P4 Rh2'
_chemical_formula_sum            'C114 H162 O2 P4 Rh2'
_chemical_formula_weight         1894.14
_chemical_melting_point          413
_chemical_name_common            'complex 2'
_chemical_properties_physical    air-sensitive
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.493(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.318(6)
_cell_length_b                   16.990(6)
_cell_length_c                   19.833(7)
_cell_measurement_reflns_used    13457
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0222
_cell_volume                     5324(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Saturn70 CCD (4x4 bin mode)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41918
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.25
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.9439
_exptl_absorpt_correction_T_min  0.9439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Higashi
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         12123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0812
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+6.6273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                10491
_reflns_number_total             12123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010799_si_001.cif
_cod_data_source_block           complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068764