Synthesis and Structural Characterization of Trinuclear CuII-Pyrazolato Complexes Containing μ3-OH, μ3-O, and μ3-Cl Ligands. Magnetic Susceptibility Study of [PPN]2[(μ3-O)Cu3(μ-pz)3Cl3]
Panagiotis A. Angaridis; Peter Baran; R. Boča; Francisco Cervantes-Lee; W. Haase; Gellert Mezei; Raphael G. Raptis; R. Werner; Inorganic Chemistry 41 (2002) 2219–2228; doi:10.1021/ic010670l

data_4317838
_publ_section_title
;
 Synthesis and Structural Characterization of Trinuclear CuII-Pyrazolato
 Complexes Containing \m3-OH, \m3-O, and \m3-Cl Ligands. Magnetic
 Susceptibility Study of [PPN]2[(\m3-O)Cu3(\m-pz)3Cl3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2219
_journal_page_last               2228
_journal_paper_doi               10.1021/ic010670l
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         Et3NH[Cu3(mu-OH)(mu-pz)3Cl3(pzH)]
_chemical_formula_sum            'C18 H30 Cl3 Cu3 N9 O'
_chemical_formula_weight         685.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.475(3)
_cell_angle_beta                 64.279(3)
_cell_angle_gamma                80.183(3)
_cell_formula_units_Z            2
_cell_length_a                   11.498(2)
_cell_length_b                   11.499(2)
_cell_length_c                   12.186(2)
_cell_measurement_temperature    298(2)
_cell_volume                     1330.9(4)
_computing_cell_refinement       'BRUKER SMART-NT V5.0'
_computing_data_collection       'BRUKER SMART-NT V5.0'
_computing_data_reduction        'BRUKER SAINT-NT V5/6.0'
_computing_molecular_graphics    'BRUKER SHELXTL-NT V5.1'
_computing_publication_material  'BRUKER SHELXTL-NT V5.1'
_computing_structure_refinement  'BRUKER SHELXTL-NT V5.1'
_computing_structure_solution    'BRUKER SHELXTL-NT V5.1'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS SMART 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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5792
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    2.706
_exptl_absorpt_correction_T_max  0.6553
_exptl_absorpt_correction_T_min  0.4595
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'plum blue'
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3815
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          2.037
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                2717
_reflns_number_total             3815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010670l.cif
_cod_data_source_block           pba018
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        1331.0(5)
_cod_database_code               4317838