Sulfate-bridged dimeric trinuclear copper(II)–pyrazolate complex with three different terminal ligands
Mezei, Gellert; Acta Crystallographica Section E Crystallographic Communications 72 (2016) 1064–; doi:10.1107/S2056989016010719

data_2020548
_publ_section_title
;
 Sulfate-bridged dimeric trinuclear copper(II)--pyrazolate complex with
 three different terminal ligands
;
_journal_coeditor_code           GK2663
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1064
_journal_paper_doi               10.1107/S2056989016010719
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Cu6 (O H)2 (S O4)2 (C3 H2 Cl N2)6 (C3 H7 N O)2 (H2 O)2], 4C3 H7 N O, 2H2 O'
_chemical_formula_moiety
'C24 H32 Cl6 Cu6 N14 O14 S2, 4(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C36 H64 Cl6 Cu6 N18 O20 S2'
_chemical_formula_weight         1727.11
_chemical_name_systematic
;Diaquahexakis(\m-4-chloropyrazolato-\k^2^<i>N</i>:<i>N</i>')bis(<i>N</i>,<i>N</i>-dimethylformamide)di-\m~3~-hydroxido-bis(\m~4~-sulfato-\k^4^<i>O</i>:<i>O</i>':<i>O</i>'':<i>O</i>'')hexacopper(II)
<i>N</i>,<i>N</i>-dimethylformamide tetrasolvate dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 109.7740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.70380(10)
_cell_length_b                   16.5265(2)
_cell_length_c                   16.6830(2)
_cell_measurement_reflns_used    6640
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.94
_cell_measurement_theta_min      2.59
_cell_volume                     3296.05(7)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.718
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_correction_T_min  0.6100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       prism
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.515
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8504
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+1.2380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                6351
_reflns_number_total             8504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gk2663sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3296.05(6)
_cod_database_code               2020548
_cod_database_fobs_code          2020548
_shelx_estimated_absorpt_t_min   0.610
_shelx_estimated_absorpt_t_max   0.894
_shelx_hkl_checksum              52625
_shelx_res_checksum              77577
_shelxl_version_number           2014/6