Conversion of some substituted phenols to the corresponding masked thiophenols, synthesis of a dinickel(II) dithiolate macrocyclic complex and isolation of some metal- and ligand-based oxidation products
Brooker, Sally; Caygill, Graham B.; Croucher, Paul D.; Davidson, Tony C.; Clive, Derrick L. J.; Magnuson, Stephen R.; Cramer, Stephen P.; Ralston, Corie Y.; Journal of the Chemical Society, Dalton Transactions  (2000) 3113–; doi:10.1039/b004214p

data_7702433
_publ_section_title
;
 Conversion of some substituted phenols to the corresponding masked
 thiophenols, synthesis of a dinickel(II) dithiolate macrocyclic complex
 and isolation of some metal- and ligand-based oxidation products
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3113
_journal_paper_doi               10.1039/b004214p
_journal_year                    2000
_chemical_formula_sum            'C31 H41.5 Cl2 N4 Ni2 O8.75 S2'
_chemical_formula_weight         862.62
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.517(2)
_cell_length_b                   27.241(3)
_cell_length_c                   15.7733(17)
_cell_measurement_temperature    158(2)
_cell_volume                     8815.8(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART area detector '
_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  0.1189
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55909
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   Semi-empirical(SADABS)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3580
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.430
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.1927
_refine_ls_R_factor_gt           0.1374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1664P)^2^+114.5085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3812
_refine_ls_wR_factor_ref         0.4096
_reflns_number_gt                4607
_reflns_number_total             7768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004214p.txt
_cod_data_source_block           tnis1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' 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.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        8815.6(17)
_cod_original_sg_symbol_H-M      Pbcn
_cod_original_formula_sum        'C31 H41.50 Cl2 N4 Ni2 O8.75 S2'
_cod_database_code               7702433