A pentanuclear complex exhibiting two short Ni‒Cu distances
Robert T. Stibrany; Harvey J. Schugar; Joseph A. Potenza; Acta Crystallographica Section E 59 (2003) m630–m632; doi:10.1107/S1600536803015496

data_2202479
_publ_section_title
;
 A pentanuclear complex exhibiting two short Ni--Cu distances
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m630
_journal_page_last               m632
_journal_paper_doi               10.1107/S1600536803015496
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu3 Ni2 Cl3 (C14 H28 N2 S2)2], 2C3 H7 N O'
_chemical_formula_moiety         'C28 H56 Cl3 Cu3 N4 Ni2 S4, 2C3 H7 N O'
_chemical_formula_sum            'C34 H70 Cl3 Cu3 N6 Ni2 O2 S4'
_chemical_formula_weight         1137.61
_chemical_name_systematic
;
 Rac-bis[(1S,2S)-trans-3,3'-(1,2-cyclohexanediyldinitrilo)bis-
(2-methylpropane-2-thiolato)]-1\k^4^N^1^,N^1'^,S^1^,S^1'^;-
2\k^4^N^2^,N^2'^,S^2^,S^2'^;3\k^2^S^1^,S^2'^;4\k^2^S^1'^,S^2^;-
5\k^2^S^1'^,S^2'^-trichloro-3\kCl,4\kCl,5\kCl-tricopper(I)-
dinickel(II) bis(dimethylformamide) solvate
;
_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                 100.480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.874(3)
_cell_length_b                   20.058(4)
_cell_length_c                   21.348(5)
_cell_measurement_reflns_used    957
_cell_measurement_temperature    223.0(10)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      3.01
_cell_volume                     5000(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP32 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223.0(10)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12812
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            'dark orange--brown'
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0545P)^2^+0.1342P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                3522
_reflns_number_total             4350
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6246.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_cell_volume        4999.4(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202479
_cod_database_fobs_code          2202479