Cyclo-[Ni(μ~2~-SPh)~2~]~9~ and cyclo-[Ni(μ~2~-SPh)~2~]~11~: new oligomeric types of toroidal nickel(ii) thiolates containing geometrically unprecedented 9- and 11-membered ring systems
Ivanov, Sergei A.; Kozee, Michael A.; Alex Merrill, W.; Agarwal, Sorabh; Dahl, Lawrence F.; Journal of the Chemical Society, Dalton Transactions  (2002) 4105–4115; doi:10.1039/b204273h

data_7011812
_publ_section_title
;
 Cyclo-[Ni(\m~2~-SPh)~2~]~9~ and cyclo-[Ni(\m~2~-SPh)~2~]~11~: new oligomeric
 types of toroidal nickel(ii) thiolates containing geometrically
 unprecedented 9- and 11-membered ring systems
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4105
_journal_page_last               4115
_journal_paper_doi               10.1039/b204273h
_journal_year                    2002
_chemical_formula_sum            'C36 H180 Ni9 O S18'
_chemical_formula_weight         1735.27
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.0237(11)
_cell_length_b                   18.0237(11)
_cell_length_c                   21.1181(19)
_cell_measurement_reflns_used    6795
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      1.62
_cell_volume                     5941.2(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  4585
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2852
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count N/A
_diffrn_standards_interval_time  N/A
_diffrn_standards_number         N/A
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  0.8464
_exptl_absorpt_correction_T_min  0.5452
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Empirical with SADABS  (Blessing, 1995)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.970
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+4.9993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                2095
_reflns_number_total             2852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204273h.txt
_cod_data_source_block           dahl126
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-31c
_cod_database_code               7011812