Controlled Formation of Tri- and Octanuclear Benzylthiolate Complexes of Zinc
Rainer Burth; Michael Gelinsky; Heinrich Vahrenkamp; Inorganic Chemistry 37 (1998) 2833–2836; doi:10.1021/ic971402j

data_4322810
_publ_section_title
;
 Controlled Formation of Tri- and Octanuclear Benzylthiolate Complexes of
 Zinc
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2833
_journal_page_last               2836
_journal_paper_doi               10.1021/ic971402j
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        Acetonitrile
_chemical_formula_sum            'C64 H66 N6 S7 Zn3'
_chemical_formula_weight         1339.76
_chemical_melting_point          134
_chemical_name_systematic
;
[{Bis(1-methyl-benzimidazol-2-ylmethyl)sulfid}-bis(benzylthiolato)-
tetrakis(mu2-benzylthiolato)-trizinc]
;
_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                90.249(15)
_cell_angle_beta                 91.866(14)
_cell_angle_gamma                95.684(15)
_cell_formula_units_Z            2
_cell_length_a                   13.550(2)
_cell_length_b                   15.313(3)
_cell_length_c                   15.493(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3197.1(10)
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.2028
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11150
_diffrn_reflns_theta_max         24.58
_diffrn_reflns_theta_min         2.46
_diffrn_standards_interval_count 'ICR every 3600 s, OCR every 200 refl.'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      1.31
_exptl_crystal_description       Isometric
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_hydrogen_treatment    Riding-Model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         10684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.2311
_refine_ls_R_factor_obs          0.0742
_refine_ls_shift/esd_max         0.036
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+30.4113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2656
_refine_ls_wR_factor_obs         0.1695
_reflns_number_observed          4934
_reflns_number_total             10713
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971402j_1.cif
_cod_data_source_block           C64H66N6S7Zn3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+30.4113P] 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^)+(0.0835P)^2^+30.4113P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322810