Effect of the Semirigid Capping Ligand on the Structure Formation of Cyano-Bridged Bimetallic Assemblies: Syntheses, Crystal Structures, and Magnetic Properties
Chen, Xiao-Yan; Shi, Wei; Xia, Jun; Cheng, Peng; Zhao, Bin; Song, Hai-Bin; Wang, Hong-Gen; Yan, Shi-Ping; Liao, Dai-Zheng; Jiang, Zong-Hui; Inorganic Chemistry 44 (2005) 4263–4269; doi:10.1021/ic050099g

data_4331490
_publ_section_title
;
 Effect of the Semirigid Capping Ligand on the Structure Formation of
 Cyano-Bridged Bimetallic Assemblies:&#x00A0; Syntheses, Crystal
 Structures, and Magnetic Properties
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4263
_journal_page_last               4269
_journal_paper_doi               10.1021/ic050099g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C54 H55 Co2 N36 Ni3 O3.5'
_chemical_formula_weight         1558.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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            4
_cell_length_a                   12.800(5)
_cell_length_b                   12.800(5)
_cell_length_c                   42.80(3)
_cell_measurement_reflns_used    930
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.25
_cell_volume                     7012(6)
_computing_cell_refinement       'Bruker SMART'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.1327
_diffrn_reflns_av_sigmaI/netI    0.1005
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            34850
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.621144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         5981
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+26.1189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1662
_reflns_number_gt                4637
_reflns_number_total             5981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050099gsup1.cif
_cod_data_source_block           040120d
_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:

'_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      P4(3)2(1)2
_cod_database_code               4331490