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_7702387
_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 N8 Ni2 S4'
_chemical_formula_weight         650.36
_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                   12.6250(10)
_cell_length_b                   14.8910(10)
_cell_length_c                   16.2020(10)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.51
_cell_measurement_theta_min      13.96
_cell_volume                     3046.0(4)
_computing_cell_refinement       'STADI4 (STOE, 1994)'
_computing_data_collection       'STADI4 (STOE, 1994)'
_computing_data_reduction        'X-RED  (STOE, 1994)'
_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      296(2)
_diffrn_measurement_device       'Siemens STOE AED2 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 1.40 - 1.58, 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       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2671
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        2.6
_diffrn_standards_interval_time  45
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  0.3730
_exptl_absorpt_correction_T_min  0.2572
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.029
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.029
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_obs          0.0461
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.00P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0900
_refine_ls_wR_factor_obs         0.0753
_reflns_number_observed          1683
_reflns_number_total             2671
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902015b.txt
_cod_data_source_block           compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Psi-Scan' was
changed to 'psi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.00P] 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^)+(0.0339P)^2^+0.00P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7702387