Two Heptacopper(II) Disk Complexes with a [Cu7(μ3-OH)4(μ-OR)2]8+ Core
James J. Henkelis; Leigh F. Jones; Marcelo P. de Miranda; Colin A. Kilner; Malcolm A. Halcrow; Inorganic Chemistry 49 (2010) 11127–11132; doi:10.1021/ic1020093

data_4317258
_publ_section_title
;
 Two Heptacopper(II) Disk Complexes with a [Cu7(\m3-OH)4(\m-OR)2]8+ Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11127
_journal_page_last               11132
_journal_paper_doi               10.1021/ic1020093
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C74 H94 Cu7 N18 O6, Cl2, 5.7[C H2 Cl2]'
_chemical_formula_sum            'C79.7 H105.4 Cl13.4 Cu7 N18 O6'
_chemical_formula_weight         2331.43
_chemical_name_systematic
; 
Hexakis[3{5}-(pyrid-2-yl)-5{3}-(tertbutyl)pyrazolido]tetrahydroxo-
dimethoxo-heptacopper(II) dichloride dichloromethane 
solvate (6/5.7)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   30.7871(3)
_cell_length_b                   30.7871(3)
_cell_length_c                   27.0562(4)
_cell_measurement_reflns_used    63739
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.07
_cell_volume                     22209.3(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method       '\w and \f 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  0.0969
_diffrn_reflns_av_sigmaI/netI    0.0893
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            63739
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Using multiple and symmetry-related data measurements via the program SORTAV
 See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            turquoise
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             10696
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.502
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         11287
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2269
_reflns_number_gt                6316
_reflns_number_total             11287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1020093_si_003.cif
_cod_data_source_block           lfj59e(Compound3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C79.70 H105.40 Cl13.40 Cu7 N18 O6'
_cod_database_code               4317258