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_4300014
_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            'C54 H48 Br Cu3 F12 N9 O3 P2'
_chemical_formula_weight         1431.50
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      173
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_audit_creation_date             'Thu Jan  8 16:09:23 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.260(2)
_cell_length_b                   14.2602
_cell_length_c                   17.693(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     3115.9(7)
_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      -0.01640
_diffrn_orient_matrix_UB_12      -0.07685
_diffrn_orient_matrix_UB_13      0.00135
_diffrn_orient_matrix_UB_21      0.07903
_diffrn_orient_matrix_UB_22      0.02523
_diffrn_orient_matrix_UB_23      -0.00434
_diffrn_orient_matrix_UB_31      0.00648
_diffrn_orient_matrix_UB_32      0.00379
_diffrn_orient_matrix_UB_33      0.05634
_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  0.057
_diffrn_reflns_av_sigmaI/netI    0.052
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2763
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        -0.27
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.793
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   '\DF (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            blue
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_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
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_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.450
_refine_diff_density_max         1.53
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     212
_refine_ls_number_reflns         1689
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0693
_refine_ls_shift/esd_max         5.0090
_refine_ls_shift/esd_mean        0.0980
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0876
_reflns_number_observed          1689
_reflns_number_total             2478
_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 

The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'hexgonal' was replaced with
'hexagonal' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 63 '
_cod_original_formula_sum        'C54 H48 Br Cu3 F12 N9 O3 P2 '
_cod_database_code               4300014