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_7011256
_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            'C40 H36 B4 F16 N14 Ni2'
_chemical_formula_weight         1177.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.880(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.177(2)
_cell_length_b                   20.579(3)
_cell_length_c                   20.410(3)
_cell_measurement_reflns_used    1451
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.43
_cell_measurement_theta_min      2.57
_cell_volume                     5494.7(14)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0790
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27961
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         9648
_refine_ls_number_restraints     560
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1937
_reflns_number_gt                5889
_reflns_number_total             9648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109526a.txt
_cod_data_source_block           '[Ni2L3(BF4)4]'
_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_cell_volume        5494.6(16)
_cod_original_sg_symbol_H-M      'P21/c  '
_cod_database_code               7011256