Heptapyridinebis(μ-dimethylglyoximato)tricopper(II) diperchlorate: a novel trinuclear copper complex bridged by glyoximate groups
Li, Chun Hui; Wang, Ru-Ji; Kou, Hui-Zhong; Li, Yadong; Acta Crystallographica Section E 59 (2003) m608–m610; doi:10.1107/S160053680301331X

data_2202775
_publ_section_title
;
 Heptapyridinebis(\m-dimethylglyoximato)tricopper(II) diperchlorate: a
 novel trinuclear copper complex bridged by glyoximate groups
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m608
_journal_page_last               m610
_journal_paper_doi               10.1107/S160053680301331X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu3 (C4 H6 N2 O2)2 (C5 H5 N)7] (Cl O4)2'
_chemical_formula_moiety         'C43 H47 Cu3 N11 O4 2+, 2Cl O4 1-'
_chemical_formula_structural     'Cu3 (C5 H5 N)7 (C4 H6 N2 O2)2 (Cl O4)2'
_chemical_formula_sum            'C43 H47 Cl2 Cu3 N11 O12'
_chemical_formula_weight         1171.47
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 104.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.615(5)
_cell_length_b                   8.3158(17)
_cell_length_c                   25.469(5)
_cell_measurement_reflns_used    3680
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.6
_cell_volume                     5047.7(19)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SMART (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '15\\times15 microns'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19837
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.428
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.639
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         7345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w = {exp[1.50(sin\q/\l)^2^]}/[\s^2^(Fo^2^)+(0.001P)^2^]
where P = (Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                2919
_reflns_number_total             7370
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6252.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202775
_cod_database_fobs_code          2202775