Regio- and chemoselective oxidation of the bis(bidentate) phosphine cis,trans,cis-1,2,3,4-tetrakis(diphenylphosphino)cyclobutane via cobalt(II) mediated dioxygen activation
Fessler, Markus; Eller, Sylvia; Bachmann, Christian; Gutmann, Rene; Trettenbrein, Barbara; Kopacka, Holger; Mueller, Thomas; Brueggeller, Peter; Dalton Transactions  (2009) 1383–; doi:10.1039/b813720j

data_7000517
_publ_section_title
;
 Regio- and chemoselective oxidation of the bis(bidentate) phosphine
 cis,trans,cis-1,2,3,4-tetrakis(diphenylphosphino)cyclobutane via
 cobalt(II) mediated dioxygen activation
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1383
_journal_paper_doi               10.1039/b813720j
_journal_year                    2009
_chemical_formula_moiety         'C52 H44 Br4 Co2 O2 P4, 2(C H Cl3)'
_chemical_formula_sum            'C54 H46 Br4 Cl6 Co2 O2 P4'
_chemical_formula_weight         1501.01
_chemical_name_common            (Co2Br4(2,3-trans-dppcbO2))
_chemical_name_systematic        '[Co2Br4(2,3-trans-dppcbO2)]'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 119.84(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.145(5)
_cell_length_b                   23.251(4)
_cell_length_c                   13.880(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     5919(2)
_computing_cell_refinement       'Software of the Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        'Software of the Siemens P4'
_computing_molecular_graphics    'SHELXTL-NT V6.1'
_computing_publication_material  'SHELXTL-NT V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega-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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7361
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.679
_exptl_absorpt_correction_T_max  0.229
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Empirical Absorption Corrections'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.430
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.2135
_reflns_number_gt                1932
_reflns_number_total             6520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813720j.txt
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7000517
_diffrn_measured_fraction        0.981