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_4317257
_publ_section_title
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 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         'C76 H92 Cu7 F6 N18 O6, 2[B F4], 2[C4 H10 O]'
_chemical_formula_sum            'C84 H112 B2 Cu7 F14 N18 O8'
_chemical_formula_weight         2234.32
_chemical_name_systematic
; 
Hexakis[3{5}-(pyrid-2-yl)-5{3}-(tertbutyl)pyrazolido]tetrahydroxo-
bis(2,2,2-trifluoroethanolato)heptacopper(II) ditetrafluoroborate 
bis-diethyl ether solvate
;
_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                116.003(3)
_cell_angle_beta                 100.297(4)
_cell_angle_gamma                92.519(4)
_cell_formula_units_Z            1
_cell_length_a                   11.1372(8)
_cell_length_b                   15.6751(11)
_cell_length_c                   16.6996(12)
_cell_measurement_reflns_used    50436
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.07
_cell_volume                     2553.3(3)
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_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 '120 microns'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50436
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1145
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         11516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0684P)^2^+4.1588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                7982
_reflns_number_total             11516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1020093_si_002.cif
_cod_data_source_block           jjh9(Compound2)
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
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_cod_database_code               4317257