<i>cyclo</i>-Tetrakis(μ-3-acetyl-4-methyl-1<i>H</i>-pyrazole-5-carboxylato-κ^4^<i>N</i>^2^,<i>O</i>^3^:<i>N</i>^1^,<i>O</i>^5^)tetrakis[aquacopper(II)] tetradecahydrate
Malinkin, Sergey; Golenya, Irina A.; Pavlenko, Vadim A.; Haukka, Matti; Iskenderov, Turganbay S.; Acta Crystallographica Section E 67 (2011) m1260–m1261; doi:10.1107/S1600536811030832

data_2231570
_publ_section_title
;
 <i>cyclo</i>-Tetrakis(\m-3-acetyl-4-methyl-1<i>H</i>-pyrazole-5-carboxylato-\k^4^<i>N</i>^2^,<i>O</i>^3^:<i>N</i>^1^,<i>O</i>^5^)tetrakis[aquacopper(II)]
 tetradecahydrate
;
_journal_coeditor_code           JH2318
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1260
_journal_page_last               m1261
_journal_paper_doi               10.1107/S1600536811030832
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cu4 (C7 H6 N2 O3)4 (H2 O)4], 14H2 O'
_chemical_formula_moiety         'C28 H32 Cu4 N8 O16, 14(H2 O)'
_chemical_formula_sum            'C28 H60 Cu4 N8 O30'
_chemical_formula_weight         1243.00
_chemical_name_systematic
;
<i>cyclo</i>-Tetrakis(\m-3-acetyl-4-methyl-1<i>H</i>-pyrazole-5-carboxylato-
\k^4^<i>N</i>^2^,<i>O</i>^3^:<i>N</i>^1^,<i>O</i>^5^)tetrakis[aquacopper(II)]
tetradecahydrate
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8502(7)
_cell_length_b                   13.8502(7)
_cell_length_c                   26.280(3)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.28
_cell_measurement_theta_min      2.59
_cell_volume                     5041.2(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
'62mm x 62mm CCD camera on three-circle goniostat'
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  'flat graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            37816
_diffrn_reflns_theta_full        30.93
_diffrn_reflns_theta_max         30.93
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.762
_exptl_absorpt_correction_T_max  0.7780
_exptl_absorpt_correction_T_min  0.5775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.581
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         3993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+11.3899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3254
_reflns_number_total             3993
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jh2318.cif
_cod_data_source_block           I
_cod_original_cell_volume        5041.1(6)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2231570
_cod_database_fobs_code          2231570