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_4300012
_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            'C63 H60 Br Cu3 F12 N9 O3 P2'
_chemical_formula_weight         1551.70
_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             'Thu Jan  8 15:44:06 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                   24.413(3)
_cell_length_b                   24.413(3)
_cell_length_c                   24.413(3)
_cell_measurement_reflns_used    13
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      29.7
_cell_volume                     14550(3)
_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      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00365
_diffrn_orient_matrix_UB_12      -0.02406
_diffrn_orient_matrix_UB_13      0.03295
_diffrn_orient_matrix_UB_21      -0.00974
_diffrn_orient_matrix_UB_22      -0.03264
_diffrn_orient_matrix_UB_23      -0.02275
_diffrn_orient_matrix_UB_31      0.03962
_diffrn_orient_matrix_UB_32      -0.00581
_diffrn_orient_matrix_UB_33      -0.00863
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  filter
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2601
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         55.06
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        -0.43
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.756
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             6280.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.26
_refine_diff_density_min         -0.82
_refine_ls_extinction_coef       0.0011(4)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_obs   1.275
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    10
_refine_ls_number_parameters     242
_refine_ls_number_reflns         1361
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0680
_refine_ls_shift/esd_max         0.0183
_refine_ls_shift/esd_mean        0.0041
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(Fo) + 0.00545|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0982
_reflns_number_observed          1361
_reflns_number_total             1671
_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:

'_refine_ls_weighting_scheme' value 'w = 1/\s^2^(Fo) +
0.00545|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/\s^2^(Fo) + 0.00545|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        14550(4)
_cod_original_sg_symbol_H-M      'I 2 3 '
_cod_original_formula_sum        'C63 H60 Br Cu3 F12 N9 O3 P2 '
_cod_database_code               4300012