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_4504497
_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
'C52 H48 N19 Ni2 O4, 2(B F4), O4 S, 4(H2 O), 4(C H4 O)'
_chemical_formula_structural
'2(Ni 2+), 2(C26 H20 N8), 2(B F4 -), O4 S 2-, 8(H2 O), 4(C H4 O)'
_chemical_formula_sum            'C56 H72 B2 F8 N16 Ni2 O16 S'
_chemical_formula_weight         1540.33
_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                109.508(10)
_cell_angle_beta                 107.144(9)
_cell_angle_gamma                90.923(9)
_cell_formula_units_Z            2
_cell_length_a                   13.818(8)
_cell_length_b                   16.645(8)
_cell_length_c                   20.937(11)
_cell_measurement_reflns_used    1054
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.98
_cell_measurement_theta_min      3.22
_cell_volume                     4302(4)
_computing_cell_refinement       SMART
_computing_data_collection       'BRUKER SMART, 1998'
_computing_data_reduction        'BRUKER SAINT, 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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.1689
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24715
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         2.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.717342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 1996'
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         17324
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.2487
_refine_ls_R_factor_gt           0.1125
_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^)+(0.1839P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2745
_refine_ls_wR_factor_ref         0.3636
_reflns_number_gt                6460
_reflns_number_total             17324
_reflns_threshold_expression     I>2s\(I)
_cod_data_source_file            cg050210tsi20051104_022830.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' 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_sg_symbol_H-M      P-1
_cod_database_code               4504497