Synthesis and crystal structure of a triangular nickel(II) complex with the shortest imine-based rigid ligand
Guo Dong; Duan Chun-ying; Fang Chen-jie; Meng Qing-jin; J. Chem. Soc., Dalton Trans.  (2002) 834–836; doi:10.1039/b109526a

data_7011255
_publ_section_title
;
 Synthesis and crystal structure of a triangular nickel(II) complex
 with the shortest imine-based rigid ligand
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              834
_journal_page_last               836
_journal_paper_doi               10.1039/b109526a
_journal_year                    2002
_chemical_formula_sum            'C46 H36 N20 Ni3 S6'
_chemical_formula_weight         1237.44
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.003(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.671(5)
_cell_length_b                   15.275(5)
_cell_length_c                   22.405(6)
_cell_measurement_reflns_used    1437
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.85
_cell_measurement_theta_min      2.49
_cell_volume                     5601(3)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1623
_diffrn_reflns_av_sigmaI/netI    0.1885
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22705
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            DARK-RED
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         7312
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_gt           0.0726
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1390
_reflns_number_gt                3343
_reflns_number_total             7312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109526a.txt
_cod_data_source_block           '[NiL(SCN)]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 
;
_cod_original_sg_symbol_H-M      'P21/n  '
_cod_database_code               7011255