The effect of N-methylation on the chemical reactivity of binuclear Ni amine-thiophenolate complexes
Kersting, Berthold; Steinfeld, Gunther; Chemical Communications  (2001) 1376–; doi:10.1039/b103050g

data_7114727
_publ_section_title
;
 The effect of N-methylation on the chemical reactivity of binuclear Ni
 amine-thiophenolate complexes
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1376
_journal_paper_doi               10.1039/b103050g
_journal_year                    2001
_chemical_compound_source
;
Crystals were grown by recrystallization from methanol
;
_chemical_formula_sum            'C63 H89 B N6 Ni2 O2 S2'
_chemical_formula_weight         1154.75
_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
_cell_angle_alpha                103.24(3)
_cell_angle_beta                 97.42(3)
_cell_angle_gamma                98.09(3)
_cell_formula_units_Z            2
_cell_length_a                   13.734(3)
_cell_length_b                   14.093(3)
_cell_length_c                   18.094(4)
_cell_measurement_temperature    180(2)
_cell_volume                     3327.5(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       'BRUKER SMART CCD'
_diffrn_measurement_method       multirun
_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  0.0959
_diffrn_reflns_av_sigmaI/netI    0.3313
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30866
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.699
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.853
_refine_ls_goodness_of_fit_obs   1.332
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         15786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.853
_refine_ls_restrained_S_obs      1.332
_refine_ls_R_factor_all          0.2617
_refine_ls_R_factor_obs          0.0893
_refine_ls_shift/esd_max         -0.056
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3036
_refine_ls_wR_factor_obs         0.2381
_reflns_number_observed          4271
_reflns_number_total             15786
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b103050g.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not determined' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1349P)^2^+0.0000P] 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^)+(0.1349P)^2^+0.0000P] 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        3327.5(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114727