Extended structures of polyiodide salts of transition metal macrocyclic complexes
Blake, Alexander J.; Li, Wan-Sheung; Lippolis, Vito; Parsons, Simon; Schröder, Martin; Acta Crystallographica Section B 63 (2007) 81–92; doi:10.1107/S0108768106041668

data_2102690
_publ_section_title
;
 Extended structures of polyiodide salts of transition metal
 macrocyclic complexes
;
_journal_coeditor_code           GP5013
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              81
_journal_page_last               92
_journal_paper_doi               10.1107/S0108768106041668
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety         'Co(C6 H12 S3)2 3+, 3(I3 -), I2'
_chemical_formula_sum            'C12 H24 Co I11 S6'
_chemical_formula_weight         1815.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.67(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.156(2)
_cell_length_b                   17.772(4)
_cell_length_c                   13.106(6)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16.75
_cell_measurement_theta_min      14.05
_cell_volume                     3506.2(19)
_computing_cell_refinement       'Stadi4 (Stoe & Cie, 1996a)'
_computing_data_collection       'Stadi4 (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material
'enCIFer (Allen et al., 2004; PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       '\w-\q, profile learning'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       -6
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_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.71
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_diffrn_standards_interval_time  60
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_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.38
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_refine_ls_extinction_coef       0.00016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3075
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_refine_ls_R_factor_all          0.0417
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.05P)^2^+91.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.103
_refine_ls_wR_factor_ref         0.108
_reflns_number_gt                2826
_reflns_number_total             3075
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gp5013.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.05P)^2^+91.0P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.05P)^2^+91.0P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3506.2(18)
_cod_database_code               2102690
_cod_database_fobs_code          2102690