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_2102692
_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         'C12 H24 Ni S6 2+, 2(I5 -)'
_chemical_formula_sum            'C12 H24 I10 Ni S6'
_chemical_formula_weight         1688.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_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           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.317(3)
_cell_length_b                   15.602(6)
_cell_length_c                   18.302(7)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.5
_cell_measurement_theta_min      14
_cell_volume                     3517(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_sigmaI/netI    0.022
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3483
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        'random variation +-3.4'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.692
_exptl_absorpt_correction_T_max  0.236
_exptl_absorpt_correction_T_min  0.145
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1996b)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    3.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.60
_refine_diff_density_min         -1.02
_refine_ls_extinction_coef       0.00023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.31
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.31
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0382
_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^)+(0.040P)^2^+25.87P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.100
_reflns_number_gt                2730
_reflns_number_total             3086
_reflns_threshold_expression     I>2\s(I)
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_cod_database_fobs_code          2102692