A Cu(II)-Mediated C-H Oxygenation of Sterically Hindered Tripyridine Ligands To Form Triangular Cu(II)3 Complexes
Masahito Kodera; Yoshimitsu Tachi; Toshio Kita; Hiromu Kobushi; Yoshinori Sumi; Koji Kano; Motoo Shiro; Masayuki Koikawa; Tadashi Tokii; Masaaki Ohba; Hisashi Okawa; Inorganic Chemistry 39 (2000) 226–234; doi:10.1021/ic990331g

data_4300015
_publ_section_title
;
A Cu(II)-Mediated C-H Oxygenation of Sterically Hindered Tripyridine
Ligands To Form Triangular Cu(II)3 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              226
_journal_page_last               234
_journal_paper_doi               10.1021/ic990331g
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C60 H54 Cl Cu3 F12 N9 O3 P2'
_chemical_formula_weight         1465.16
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      197
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_audit_creation_date             'Fri Jan  9 13:05:21 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.177(3)
_cell_length_b                   24.1765
_cell_length_c                   24.1765
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     14131.5(18)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00054
_diffrn_orient_matrix_UB_12      -0.02303
_diffrn_orient_matrix_UB_13      -0.03436
_diffrn_orient_matrix_UB_21      0.00102
_diffrn_orient_matrix_UB_22      -0.03434
_diffrn_orient_matrix_UB_23      0.02303
_diffrn_orient_matrix_UB_31      -0.04135
_diffrn_orient_matrix_UB_32      -0.00114
_diffrn_orient_matrix_UB_33      0.00012
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_av_sigmaI/netI    0.102
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4511
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        -1.07
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5944.00
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.450
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.120
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    8
_refine_ls_number_parameters     211
_refine_ls_number_reflns         1445
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0716
_refine_ls_shift/esd_max         0.1660
_refine_ls_shift/esd_mean        0.0150
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0850
_reflns_number_observed          1445
_reflns_number_total             2916
_reflns_observed_criterion       >3.0sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        14131(4)
_cod_original_sg_symbol_H-M      'I 2 3 '
_cod_original_formula_sum        'C60 H54 Cl Cu3 F12 N9 O3 P2 '
_cod_database_code               4300015