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_7000523
_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 Co2 I4 O4 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C54 H48 Cl4 Co2 I4 O4 P4'
_chemical_formula_weight         1652.112
_chemical_name_common            (Co2I4(dppcbO4))
_chemical_name_systematic        '[Co2I4(dppcbO4)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.5027(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4421(2)
_cell_length_b                   20.1430(2)
_cell_length_c                   21.5066(3)
_cell_measurement_reflns_used    70821
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     6130.77(14)
_computing_cell_refinement       'Denzo and Scalepack'
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'Denzo and Scalepack'
_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      223(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'phi- and 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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37797
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Otwinowski et al, 1997'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         11879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+4.8538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                9466
_reflns_number_total             12170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813720j.txt
_cod_data_source_block           7c
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7000523
_diffrn_measured_fraction        0.982