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_7000519
_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
'2(C52 H44 Co2 I4 O3 P4), 1.8(C H2 Cl2), H2 O'
_chemical_formula_sum            'C105.8 H93.6 Cl3.6 Co4 I8 O7 P8'
_chemical_formula_weight         3103.44
_chemical_name_common            (Co2I4(dppcbO3))
_chemical_name_systematic        '[Co2I4(dppcbO3)]'
_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                93.74(3)
_cell_angle_beta                 97.49(3)
_cell_angle_gamma                110.54(3)
_cell_formula_units_Z            2
_cell_length_a                   14.491(3)
_cell_length_b                   20.193(4)
_cell_length_c                   21.528(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     5807(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      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.1264
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22104
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.931
_exptl_absorpt_correction_T_max  0.235
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Empirical Absorption Corrections'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2995.2
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.750
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         10487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2105
_refine_ls_wR_factor_ref         0.2495
_reflns_number_gt                10487
_reflns_number_total             20559
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            b813720j.txt
_cod_data_source_block           4
_cod_original_formula_sum        'C105.80 H93.60 Cl3.60 Co4 I8 O7 P8'
_cod_database_code               7000519
_diffrn_measured_fraction        0.990