Novel pyrazolate-based copper(II) [2x2] grid complexes: Synthesis, structure and properties
Malinkin, Sergej; Penkova, Larysa; Moroz, Yurii; Maciag, Anna; Haukka, Matti; Szebesczyk, Agnieszka; Kozlowski, Henryk; Gumienna-Kontecka, Elzbieta; Pavlenko, Vadim; Meyer, Franc; Nordlander, Ebbe; Fritsky, Igor; Inorganica Chimica Acta 392 (2012) 322–330; doi:10.1016/j.ica.2012.03.021

data_1512624
_publ_section_title
;
 Novel pyrazolate-based copper(II) [2x2] grid complexes: Synthesis,
 structure and properties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              322
_journal_page_last               330
_journal_paper_doi               10.1016/j.ica.2012.03.021
_journal_volume                  392
_journal_year                    2012
_chemical_formula_moiety         'C48 H44 Cu4 N12 O12, 4(H2 O)'
_chemical_formula_sum            'C48 H52 Cu4 N12 O16'
_chemical_formula_weight         1307.22
_chemical_name_systematic
;
 Tetra(3-acetyl-4-methyl-5-carboxylate-pyrazolato)-\m-pyrazolato)-
tetra(pyridine)tetra(copper(II))
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 114.120(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3907(9)
_cell_length_b                   13.5643(4)
_cell_length_c                   21.5049(9)
_cell_measurement_temperature    100(2)
_cell_volume                     5162.4(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'Diamond v.3.2c (Brandenburg, 2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device
'62mm x 62mm CCD camera on three-circle goniostat'
_diffrn_measurement_device_type  'Bruker SMART APEX II 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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            72049
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  0.8294
_exptl_absorpt_correction_T_min  0.5813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         14922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                10288
_reflns_number_total             14922
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2012-392-322-330-1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 2/n '
_cod_database_code               1512624