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_7009263
_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            'C25 H18 Cl2 Cu2 N6 S'
_chemical_formula_weight         632.49
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.142(3)
_cell_length_b                   10.625(2)
_cell_length_c                   19.535(6)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.47
_cell_measurement_theta_min      5.13
_cell_volume                     2520.1(11)
_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       '\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  0.0995
_diffrn_reflns_av_sigmaI/netI    0.1836
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3559
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.010
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.222
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         2734
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.173
_refine_ls_R_factor_all          0.1850
_refine_ls_R_factor_obs          0.0728
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1519
_refine_ls_wR_factor_obs         0.1129
_reflns_number_observed          1600
_reflns_number_total             3365
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a909604c.txt
_cod_data_source_block           compound_3
_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^)+(0.0261P)^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^)+(0.0261P)^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_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7009263