Iodide Ion Pairing with Highly Charged Ruthenium Polypyridyl Cations in CH3CN.
Swords, Wesley B.; Li, Guocan; Meyer, Gerald J.; Inorganic chemistry 54 (2015) 4512–4519; doi:10.1021/acs.inorgchem.5b00344

data_4343201
_publ_section_title
;
 Iodide Ion Pairing with Highly Charged Ruthenium Polypyridyl Cations in
 CH3CN.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4512
_journal_page_last               4519
_journal_paper_doi               10.1021/acs.inorgchem.5b00344
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C54 H84 N12 Ru, 4(F12 P2), 2(C2 H3 N)'
_chemical_formula_sum            'C58 H90 F48 N14 P8 Ru'
_chemical_formula_weight         2244.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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     iterative
_audit_creation_date             2014-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.048(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3741(7)
_cell_length_b                   30.0594(13)
_cell_length_c                   21.7725(9)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.93
_cell_measurement_theta_min      2.94
_cell_volume                     9401.4(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_laue_measured_fraction_full 0.981
_diffrn_reflns_laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75561
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.189
_diffrn_reflns_theta_min         2.940
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.920
_exptl_absorpt_correction_T_max  0.8386
_exptl_absorpt_correction_T_min  0.5286
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0736 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.6303.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       plate
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         8764
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+23.8082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6826
_reflns_number_total             8764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00344_si_002.cif
_cod_data_source_block           x1411006
_cod_database_code               4343201
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.337
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 P62, F64, F65, F66, F67, F68, F69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(F67)=Sof(F68)=Sof(F69)=1-FVAR(1)
 Sof(F64)=Sof(F65)=Sof(F66)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C15(H15A,H15B), C27(H27A,H27B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C10(H10), C13(H13), C20(H20), C21(H21), C25(H25), C32(H32),
 C33(H33)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              28613
_shelx_hkl_checksum              22726
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2014-11-24
_olex2_date_sample_submission    2014-11-19
_olex2_diffrn_ambient_temperature_device Kryoflex
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder paratone oil'
_olex2_submission_original_sample_id WS-2-Tris+TBAI
_olex2_submission_special_instructions 'No special instructions were received'