Preparation of the first sulfur-containing cobalt and nickel complexes stabilised by the macrocyclic cyclam ligand; observation of S‒H bond activation
Pleus, Rainer J.; Waden, Harald; Saak, Wolfgang; Haase, Detlev; Pohl, Siegfried; Journal of the Chemical Society, Dalton Transactions  (1999) 2601–; doi:10.1039/a902015b

data_7702386
_publ_section_title
;
 Preparation of the first sulfur-containing cobalt and nickel complexes
 stabilised by the macrocyclic cyclam ligand; observation of S--H bond
 activation
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2601
_journal_paper_doi               10.1039/a902015b
_journal_year                    1999
_chemical_formula_sum            'C20 H52 Co2 N8 S4'
_chemical_formula_weight         650.80
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_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            4
_cell_length_a                   12.482(6)
_cell_length_b                   14.699(7)
_cell_length_c                   16.045(6)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.8
_cell_measurement_theta_min      11.8
_cell_volume                     2944(2)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'SHELXTL-PC (Siemens, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-PC (Siemens, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens STOE AED2 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 2.46 - 2.58, scan ratio 2theta:omega = 0.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2304
_diffrn_reflns_theta_max         23.96
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        3.5
_diffrn_standards_interval_time  45
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.6632
_exptl_absorpt_correction_T_min  0.3734
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.262
_refine_ls_goodness_of_fit_obs   1.208
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.309
_refine_ls_restrained_S_obs      1.208
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_obs          0.0553
_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^)+(0.0511P)^2^+2.6035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1403
_refine_ls_wR_factor_obs         0.1114
_reflns_number_observed          1740
_reflns_number_total             2304
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902015b.txt
_cod_data_source_block           compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+2.6035P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+2.6035P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2943.8(23)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7702386