Complexes of ditopic carbo- and thio-carbohydrazone ligands‒mononuclear, 1D chain, dinuclear and tetranuclear examples.
Tandon, Santokh S.; Dul, Marie-Claire; Lee, John L.; Dawe, Louise N.; Anwar, Muhammad U.; Thompson, Laurence K.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 3466–3475; doi:10.1039/c0dt01487g

data_7015323
_publ_section_title
;
 Complexes of ditopic carbo- and thio-carbohydrazone
 ligands--mononuclear, 1D chain, dinuclear and tetranuclear examples.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3466
_journal_page_last               3475
_journal_paper_doi               10.1039/c0dt01487g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety
'(C36 H60 N24 Ni4 O8 S4), 4(Cl O4), 9.5(H2 O)'
_chemical_formula_sum            'C36 H78 Cl4 N24 Ni4 O33.5 S4'
_chemical_formula_weight         1888.00
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                80.500(11)
_cell_angle_beta                 77.768(15)
_cell_angle_gamma                88.138(16)
_cell_formula_units_Z            4
_cell_length_a                   15.241(3)
_cell_length_b                   22.657(5)
_cell_length_c                   24.327(4)
_cell_measurement_reflns_used    31371
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.0047
_cell_measurement_theta_min      2.4247
_cell_volume                     8097(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.1129
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            62773
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.9313
_exptl_absorpt_correction_T_min  0.8280
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 317 electrons per
unit cell in five voids (total volume 1694.4 ^A^3); that is 92.75 electrons
per formula unit. Disordered lattice solvent water molecules (approx. 9)
were present prior to the application of Squeeze, however, a good point
atom model could not be achieved. Note that one lattice solvent water
molecule, O49 was not removed via Squeeze, but rather, was left in the
model as it makes significant H-bonding interactions with ligands from
both grid moieties in the asymmetric unit. The application of Squeeze
gave a good improvement in the data statistics and allowed for a full
anisotropic refinement of the structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         1.909
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1741
_refine_ls_number_reflns         28333
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.1153
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1462P)^2^+32.7023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2965
_refine_ls_wR_factor_ref         0.3256
_reflns_number_gt                18856
_reflns_number_total             28333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01487g.txt
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Numerical' changed to 'numerical'
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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_formula_sum        'C36 H78 Cl4 N24 Ni4 O33.50 S4'
_cod_database_code               7015323