Novel square-planar cyclic tetranuclear copper(II) complex containing oximate bridges. Synthesis, crystal structure and magnetic properties of tetrakis[diaqua(μ-1,3-dimethylviolurato)copper(II)] tetraperchlorate dihydrate
Colacio, Enrique; López-Magaña, Carlos; McKee, Vickie; Romerosa, Antonio; Journal of the Chemical Society, Dalton Transactions  (1999) 2923–; doi:10.1039/a904012i

data_7027560
_publ_section_title
;
 Novel square-planar cyclic tetranuclear copper(II) complex containing
 oximate bridges. Synthesis, crystal structure and magnetic properties of
 tetrakis[diaqua(\m-1,3-dimethylviolurato)copper(II)] tetraperchlorate
 dihydrate
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2923
_journal_paper_doi               10.1039/a904012i
_journal_year                    1999
_chemical_formula_sum            'C6 H11 Cl Cu N3 O10.5'
_chemical_formula_weight         392.17
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            8
_cell_length_a                   18.761(4)
_cell_length_b                   18.761(4)
_cell_length_c                   7.524(4)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      4.5
_cell_volume                     2648.3(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1641
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown/yellow
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.78
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         1540
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.114
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+75.1807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1721
_reflns_number_gt                1335
_reflns_number_total             1540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904012isup1.cif
_cod_data_source_block           amcu2x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

data name '_atom_site_symmetry_multiplicit' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        2648.5(16)
_cod_original_formula_sum        'C6 H11 Cl Cu N3 O10.50'
_cod_database_code               7027560