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_7114725
_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            'C33 H56 Cl2 N6 Ni2 O5 S2'
_chemical_formula_weight         869.28
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.941(5)
_cell_length_b                   26.974(5)
_cell_length_c                   12.477(2)
_cell_measurement_temperature    293(2)
_cell_volume                     8057(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker SMART CCD'
_diffrn_measurement_method       hemisphere
_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  0.1201
_diffrn_reflns_av_sigmaI/netI    0.1582
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25074
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.954
_refine_ls_goodness_of_fit_obs   0.990
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8935
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.954
_refine_ls_restrained_S_obs      0.990
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_obs          0.0587
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1764
_refine_ls_wR_factor_obs         0.1289
_reflns_number_observed          4578
_reflns_number_total             8935
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b103050g.txt
_cod_data_source_block           4
_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^)+(0.0776P)^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^)+(0.0776P)^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        8057.5(26)
_cod_original_sg_symbol_H-M      Iba2
_cod_database_code               7114725