The effect of hydrogen-bonding anions on the structure of metal–sulfimide complexes
Dale, Sophie H.; Elsegood, Mark R. J.; Holmes, Kathryn E.; Kelly, Paul F.; Acta Crystallographica Section C 61 (2005) m34–m39; doi:10.1107/S0108270104029051

data_2014622
_publ_section_title
;
 The effect of hydrogen-bonding anions on the structure of
 metal--sulfimide complexes
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m34
_journal_page_last               m39
_journal_paper_doi               10.1107/S0108270104029051
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Co (C12 H11 N S)6] I2, C12 H11 N S, 2C2 H3 N'
_chemical_formula_moiety
'C72 H66 Co N6 S6 2+, 2I -, C12 H11 N S, 2C2 H3 N'
_chemical_formula_sum            'C88 H83 Co I2 N9 S7'
_chemical_formula_weight         1803.86
_chemical_name_systematic
;
Hexakis(S,S-diphenylsulfimide)cobalt(II) diiodide diphenylsulfimide
acetonitrile disolvate
;
_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
'placed geometrically except NH which were refined with restraints'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.557(2)
_cell_angle_beta                 87.490(2)
_cell_angle_gamma                78.807(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0776(6)
_cell_length_b                   15.1667(7)
_cell_length_c                   22.4675(11)
_cell_measurement_reflns_used    49288
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.30
_cell_volume                     4192.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49288
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1838
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         19601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0244P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                12795
_reflns_number_total             19601
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1594.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (6
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4192.5(3)
_cod_database_code               2014622
_cod_database_fobs_code          2014622