Self-assembled macrocyclic tetranuclear molecular square [Ni(HL)]44+ and molecular rectangle [Cu2Cl2L]2{H2L = bis[phenyl(2-pyridyl)methanone] thiocarbazone}
He Cheng; Duan Chun-ying; Fang Chen-jie; Liu Yong-jiang; Meng Qing-jin; J. Chem. Soc., Dalton Trans.  (2000) 1207–1212; doi:10.1039/a909604c

data_7009262
_publ_section_title
;
 Self-assembled macrocyclic tetranuclear molecular square [Ni(HL)]44+
 and molecular rectangle
 [Cu2Cl2L]2{H2L&#x00A0;=&#x00A0;bis[phenyl(2-pyridyl)methanone]
 thiocarbazone}
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1207
_journal_page_last               1212
_journal_paper_doi               10.1039/a909604c
_journal_year                    2000
_chemical_formula_sum            'C27 H25.5 F6 N6 Ni O1.25 P S'
_chemical_formula_weight         689.77
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.38(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   27.045(9)
_cell_length_b                   16.385(7)
_cell_length_c                   29.595(9)
_cell_measurement_temperature    293(2)
_cell_volume                     12371(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.1168
_diffrn_reflns_av_sigmaI/netI    0.3284
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8968
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        14.35
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.5871
_exptl_absorpt_correction_T_min  0.4914
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'black                 '
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       'prism                 '
_exptl_crystal_F_000             5640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.819
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_hydrogen_treatment    'riding mdoel'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         8081
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      0.822
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.2630
_refine_ls_R_factor_obs          0.0787
_refine_ls_shift/esd_max         -0.047
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2556
_refine_ls_wR_factor_obs         0.1623
_reflns_number_observed          2499
_reflns_number_total             8081
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a909604c.txt
_cod_data_source_block           compound_2
_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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        12371.6(75)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_original_formula_sum        'C27 H25.50 F6 N6 Ni O1.25 P S'
_cod_database_code               7009262