New Oxamato-Bridged Trinuclear CuII-CuII-CuII Complexes with Hydrogen-Bond Supramolecular Structures: Synthesis and Magneto-Structural Studies
Javier Tercero; Carmen Diaz; Joan Ribas; José Mahía; Miguel Angel Maestro; Inorganic Chemistry 41 (2002) 5373–5381; doi:10.1021/ic011081i

data_4318655
_publ_section_title
;
 New Oxamato-Bridged Trinuclear CuII-CuII-CuII Complexes with
 Hydrogen-Bond Supramolecular Structures: Synthesis and Magneto-Structural
 Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5373
_journal_page_last               5381
_journal_paper_doi               10.1021/ic011081i
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C21 H42 Cu3 N6 O6, P F6, C N S, 4(H2 O) '
_chemical_formula_sum            'C22 H50 Cu3 F6 N7 O10 P S'
_chemical_formula_weight         940.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.0820(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.68970(10)
_cell_length_b                   18.150
_cell_length_c                   32.1949(4)
_cell_measurement_temperature    298(2)
_cell_volume                     3909.04(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            26496
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        0.40
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.9156
_exptl_absorpt_correction_T_min  0.4673
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         9571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+5.9930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1892
_reflns_number_gt                5680
_reflns_number_total             9571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011081i_2.cif
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3909.15(8)
_cod_database_code               4318655