[Ni(L)(MeCN)][BF4]2 {L = 2,5,8-trithia[9],(2,9)-1,10-phenanthrolinophane} as a building block for the synthesis of binuclear nickel(II) complexes: X-ray crystal structure and magnetochemistry of a singly F-bridged nickel(II) dimer
Alexander J. Blake; Francesco A. Devillanova; Alessandra Garau; Andrew Harrison; Francesco Isaia; Vito Lippolis; Satish K. Tiwary; Martin Schröder; Gaetano Verani; Gavin Whittaker; J. Chem. Soc., Dalton Trans.  (2002) 4389–4394; doi:10.1039/b207934h

data_7012148
_publ_section_title
;
 [Ni(L)(MeCN)][BF4]2&#x00A0;{L =
 2,5,8-trithia[9],(2,9)-1,10-phenanthrolinophane} as a building block
 for the synthesis of binuclear nickel(II) complexes: X-ray crystal
 structure and magnetochemistry of a singly F-bridged nickel(II) dimer
;
_journal_issue                   23
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4389
_journal_page_last               4394
_journal_paper_doi               10.1039/b207934h
_journal_year                    2002
_chemical_formula_moiety         'C18 H18 N5 Ni S3 +, B F4 -'
_chemical_formula_sum            'C18 H18 B F4 N5 Ni S3'
_chemical_formula_weight         546.08
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                104.688(7)
_cell_angle_beta                 95.563(9)
_cell_angle_gamma                100.377(11)
_cell_formula_units_Z            2
_cell_length_a                   7.2069(6)
_cell_length_b                   11.0525(8)
_cell_length_c                   14.0537(8)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      13.5
_cell_volume                     1053.11(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       omega/theta
_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  0.059
_diffrn_reflns_av_sigmaI/netI    0.026
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4234
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red/brown
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.35
_refine_diff_density_rms         0.06
_refine_ls_extinction_coef       'riding model'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.041P)^2^+1.422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                3016
_reflns_number_total             3718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207934h.txt
_cod_data_source_block           NIZPNS
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (2
times).

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.041P)^2^+1.422P] 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^)+(0.041P)^2^+1.422P] 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        1053.11(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012148