Syntheses, Structure, and Properties of the Metal Complexes with 3-(2-Pyridyl)pyrazole-Based Ligands: Tuning the Complex Structures by Ligand Modifications
Zou, Ru-Qiang; Liu, Chun-Sen; Huang, Zheng; Hu, Tong-Liang; Bu, Xian-He; Crystal Growth & Design 6 (2006) 99–; doi:10.1021/cg050210t

data_4504498
_publ_section_title
;
 Syntheses, Structure, and Properties of the Metal Complexes with
 3-(2-Pyridyl)pyrazole-Based Ligands:&#x2009; Tuning the Complex
 Structures by Ligand Modifications
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              99
_journal_paper_doi               10.1021/cg050210t
_journal_volume                  6
_journal_year                    2006
_chemical_formula_moiety
'C72 H102 Cu6 N18 O18, 10(Cl O4-),2(OH-), 2(CH3CN),9(H2 O)'
_chemical_formula_structural
'6(Cu 2+), 2(C36 H33 N9), 10(Cl O4 -),2(OH-),2(CH3CN), 27(H2 O)'
_chemical_formula_sum            'C76 H128 Cl10 Cu6 N20 O69'
_chemical_formula_weight         3165.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 115.187(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.067(12)
_cell_length_b                   25.610(9)
_cell_length_c                   17.498(7)
_cell_measurement_reflns_used    1050
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.98
_cell_measurement_theta_min      3.22
_cell_volume                     13004(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART, BRUKER 1998'
_computing_data_reduction        'SAINT, BRUKER 1998''
_computing_molecular_graphics    'SHELXTL, SHELDRICK, 1997B'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997A)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997A)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'bruker ccd area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0620
_diffrn_reflns_av_sigmaI/netI    0.1298
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24255
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.877998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs; bruker, 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6500
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         12705
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.2143
_refine_ls_R_factor_gt           0.0875
_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^)+(0.1354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2107
_refine_ls_wR_factor_ref         0.2788
_reflns_number_gt                5130
_reflns_number_total             12705
_reflns_threshold_expression     I>2si\(I)
_cod_data_source_file            cg050210tsi20051104_022830.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        13003(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4504498