Hexakis-μ-chlorido-dichloridobis[(3,5-dimethylpyrazol-1-yl)acetic acid-κ^2^<i>N</i>,<i>N</i>']tetracopper(II): an unexpected neutral bis-pyrazolyl ligand in a tetracopper(II) complex
Pevec, Andrej; Kozlevčar, Bojan; Gamez, Patrick; Reedijk, Jan; Acta Crystallographica Section E 63 (2007) m514–m516; doi:10.1107/S1600536807001493

data_2212377
_publ_section_title
;
 Hexakis-\m-chlorido-dichloridobis[(3,5-dimethylpyrazol-1-yl)acetic
 acid-\k^2^<i>N</i>,<i>N</i>']tetracopper(II): an unexpected neutral
 bis-pyrazolyl ligand in a tetracopper(II) complex
;
_journal_coeditor_code           SK3091
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m514
_journal_page_last               m516
_journal_paper_doi               10.1107/S1600536807001493
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu4 Cl8 (C12 H16 N4 O2)2]'
_chemical_formula_moiety         'C24 H32 Cl8 Cu4 N8 O4'
_chemical_formula_sum            'C24 H32 Cl8 Cu4 N8 O4'
_chemical_formula_weight         1034.34
_chemical_name_systematic
;
Hexakis-\m-chloro-dichloro-bis[(3,5-dimethylpyrazol-1-yl)acetic
acid-\k^2^N,N']tetracopper(II)
;
_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                117.6094(10)
_cell_angle_beta                 98.6850(10)
_cell_angle_gamma                98.2172(16)
_cell_formula_units_Z            1
_cell_length_a                   9.3869(2)
_cell_length_b                   10.6666(2)
_cell_length_c                   10.7902(3)
_cell_measurement_reflns_used    2660
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     918.00(4)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.055
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
;
Nonius KappaCCD area-detector
;
_diffrn_measurement_method       \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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5946
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_reflns_theta_min         3.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.911
_exptl_absorpt_correction_T_max  0.7595
_exptl_absorpt_correction_T_min  0.6692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0056P)^2^+0.8188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                3395
_reflns_number_total             4088
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3091.cif
_cod_data_source_block           I
_cod_database_code               2212377
_cod_database_fobs_code          2212377