First Examples of Dinickel Complexes Containing the N3Ni(μ2-SR)3NiN3 Core. Synthesis and Crystal Structures of [L2Ni2][BPh4]2 and [L3Ni2][BPh4]2 (L = 2,6-Di(aminomethyl)-4-tert-butyl-thiophenolate)
Berthold Kersting; Dieter Siebert; Inorganic Chemistry 37 (1998) 3820–3828; doi:10.1021/ic980131p

data_4322913
_publ_contact_author
;
 Dr. Berthold Kersting
 Institut fuer Anorganische und Analytische Chemie
 Albertstr. 21
 79104 Freiburg
 Germany
;
_publ_contact_author_email       kerstber@sun2.ruf.uni-freiburg.de
_publ_contact_author_fax         '+49/(0)761/203 6001'
_publ_contact_author_phone       '+49/(0)761/203 6116'
_publ_section_title
;
 First Examples of Dinickel Complexes Containing the N3Ni(\m2-SR)3NiN3
 Core. Synthesis and Crystal Structures of [L2Ni2][BPh4]2 and
 [L3Ni2][BPh4]2 (L = 2,6-Di(aminomethyl)-4-tert-butyl-thiophenolate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3820
_journal_page_last               3828
_journal_paper_doi               10.1021/ic980131p
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        MeOH-CH3CN
_chemical_formula_structural
;        
  [(4-t-Bu-2,6(CH2NH2)2-C6H2SH)2Ni2][B(C6H5)4]2MeOHCH3CN
;
_chemical_formula_sum            'C75 H85 B2 N5 Ni2 O S2'
_chemical_formula_weight         1275.64
_chemical_melting_point          506(2)
_chemical_name_systematic
; 
 Di(2,6-di(aminomethyl)-4-tert-butyl-thiophenolato)dinickel(II)- 
 di(tetraphenylborate)-methanol-acetonitrile
;
_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                 110.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.940(4)
_cell_length_b                   13.901(3)
_cell_length_c                   23.918(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6855(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Nonius-Turbo-CAD4
_diffrn_measurement_method       Omega-2Theta
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13792
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         2.93
_diffrn_standards_interval_count 'OCR every 200 refl.'
_diffrn_standards_interval_time  'ICR every 1800 s.'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       'transparent blocks'
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          1.2
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.161
_refine_ls_goodness_of_fit_obs   1.159
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         13432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_obs          0.0580
_refine_ls_shift/esd_max         -0.202
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+5.8367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1852
_refine_ls_wR_factor_obs         0.1475
_reflns_number_observed          8937
_reflns_number_total             13460
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980131p_1.cif
_cod_data_source_block           ni2l2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'monoclinic P' was replaced with
'monoclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+5.8367P] 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^)+(0.0814P)^2^+5.8367P] 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        6854.8(24)
_cod_database_code               4322913