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_4322914
_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)
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_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
_chemical_formula_structural
;
 [(2,6(CH2NH2)2-4-t-Bu-C6H2S)3Ni2][B(C6H5)4]2MeOH
;
_chemical_formula_sum            'C85 H101 B2 N6 Ni2 O S3'
_chemical_formula_weight         1457.94
_chemical_name_systematic
; 
 Tris(2,6-di(aminomethyl)-4-tert-butyl-thiophenolato)dinickel(III,II) 
 -di(tetraphenylborate)-methanol
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 106.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.678(5)
_cell_length_b                   20.090(4)
_cell_length_c                   16.797(3)
_cell_measurement_temperature    213(2)
_cell_volume                     7674(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       STOE-IPDS
_diffrn_measurement_method
;
 STOE IPDS MEASUREMENT AND DATA EVALUATION SUMMARY for NII
 EXPOSE   Date and time                             09-Dec-97  15:17
         Wavelength [A]                                     0.71073
         (First) exposure                                         1
         Tube power [kW]                                       1.75
         Tube voltage [kV]                                       50
         Tube current [mA]                                       35
         Collimator size [mm]                                   0.5
         Temperature [K]                                      213.0
         Detector distance [mm]                                70.0
         2theta range [degrees]                        8.1     52.1
         d(hkl) range [A]                            5.013    0.809
         Phi movement mode                                 Rotation
         Phi start [degrees]                                  160.0
         Phi end   [degrees]                                  360.0
         Phi incr. [degrees]                                    1.0
         Number of exposures                                    200
         Irradiation / exposure [min]                          4.00
         Measurement duration [h]                                27

 PROFILE  Profile function                                   Dynamic
         Smallest profile diameter [pixels]                      13
         Largest  profile diameter [pixels]                      17
         Chi^2 of fit [pixels^2]                                0.1

 INTEGRATE   
         Profile function                                   Dynamic
         Smallest profile diameter [pixels]                      13
         Largest  profile diameter [pixels]                      17
         Automated overlap check?                               Yes
         Overlap tolerance [pixel]                                0
         Exposure range                                     1   182
         Control reflections                               50   200
         I/sigma limit for control reflections                  8.0
         Crystal system                                   triclinic
         Lattice type                                             P
         Initial a     [A]                                    16.80
         Initial b     [A]                                    20.08
         Initial c     [A]                                    23.68
         Initial alpha [degrees]                              90.07
         Initial beta  [degrees]                             106.18
         Initial gamma [degrees]                              90.06
         Effective mosaic spread                              0.011
         Direction cosines?                                     Yes
         q vector mode (6 indices)?                              No

         Overlapped reflections                                   0
         Overloaded reflections                                  18
         Total number of stored reflections             55230  100%
         Reflections with Fo2 > 1 * sigma(Fo2)          43061   78%
         Reflections with Fo2 > 2 * sigma(Fo2)          37605   68%
         Reflections with Fo2 > 4 * sigma(Fo2)          30233   55%
         Mean Fo2/sigma(Fo2)                                   12.8

  SELECT   Minimum input  phi [degrees]                         160.0
         Maximum input  phi [degrees]                         342.0
         Minimum output phi [degrees]                         160.0
         Maximum output phi [degrees]                         342.0

         Minimum input  2theta [degrees]                        8.9
         Maximum input  2theta [degrees]                       52.0
         Minimum output 2theta [degrees]                        8.9
         Maximum output 2theta [degrees]                       52.0

         Minimum input  I/sigma(I)                              8.0
         Maximum input  I/sigma(I)                            910.3
         Minimum output I/sigma(I)                              8.0
         Maximum output I/sigma(I)                            910.3

         Minimum input  Chi^2 [A^-2]                       0.23E-08
         Maximum input  Chi^2 [A^-2]                       0.18E-03

  CELL     Number of reflections                                 5000

         Lattice                                        triclinic P

         A           [A]                            16.7966  0.0011
         B           [A]                            20.0905  0.0013
         C           [A]                            23.6785  0.0015
         Alpha       [degrees]                       89.968   0.007
         Beta        [degrees]                      106.158   0.007
         Gamma       [degrees]                       90.055   0.007

         Volume      [A^3]                                   7674.7

         Orientation [A^-1]         -0.023258  -0.044485  -0.015005
                                     0.057037  -0.019430   0.011979
                                    -0.006921  -0.011007   0.039556

  DECAY    Correction desired. Smooth factor:                       0
         First exposure number                                    1
         Last exposure number                                   182

         Number of stored reflections                         55230
         Direction cosines                                   Stored

;
_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  0.1148
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54356
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         4.37
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3100
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.999
_refine_ls_goodness_of_fit_obs   1.025
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         14890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_restrained_S_obs      1.025
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_obs          0.0504
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+6.4051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1360
_refine_ls_wR_factor_obs         0.1202
_reflns_number_observed          11240
_reflns_number_total             14892
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980131p_2.cif
_cod_data_source_block           nii
_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^)+(0.0529P)^2^+6.4051P] 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^)+(0.0529P)^2^+6.4051P] 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        7674.5(26)
_cod_database_code               4322914