Tuning the chaotropic effect as an assembly motif through one-electron transfer in rhenium cluster
Ivanov, Anton A.; Falaise, Clément; Landy, David; Haouas, Mohamed; Mironov, Yuri V.; Shestopalov, Michael A.; Cadot, Emmanuel; Chemical Communications  (2019) –; doi:10.1039/C9CC05136H

data_7123917
_publ_section_title
;
 Tuning the chaotropic effect as an assembly motif through one-electron
 transfer in rhenium cluster
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05136H
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C6 N6 Re6 Se8, C48 H56 O40, C48 H48 O40, C48 H52 O40, 24(O)'
_chemical_formula_sum            'C150 H156 N6 O146 Re6 Se8'
_chemical_formula_weight         6127.68
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_symmetry_space_group_name_Hall  'I 4 2'
_symmetry_space_group_name_H-M   'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-28 deposited with the CCDC.    2019-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8167(14)
_cell_length_b                   23.8167(14)
_cell_length_c                   57.132(4)
_cell_measurement_reflns_used    9568
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.46
_cell_volume                     32407(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            282624
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.128
_diffrn_reflns_theta_max         25.128
_diffrn_reflns_theta_min         2.139
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.211
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1229 before and 0.0918 after correction. The Ratio of minimum to maximum transmission is 0.7503. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       plate
_exptl_crystal_F_000             11952
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.861
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.021(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         14443
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0829P)^2^+525.5223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                11917
_reflns_number_total             14443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05136h2.cif
_cod_data_source_block           iaa165_0m
_cod_original_cell_volume        32408(4)
_cod_database_code               7123917
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.566
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.021(16)
 -0.021(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C6C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9W) \\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O7W(0.5) O4W(0.5) O13W(0.25) O9W(0.5) O8W(0.5) O1W(0.5) O2W(0.5)
 O3W(0.5) O12W(0.25) O6W(0.5) O11W(0.5)
5.a Ternary CH refined with riding coordinates:
 C12A(H12A), C9A(H9A), C6A(H6A), C3C(H3C), C1B(H1B), C8A(H8A), C10B(H10B),
 C4A(H4A), C7C(H7C), C3A(H3A), C5B(H5B), C7A(H7A), C10C(H10C), C3B(H3B),
 C2A(H2A), C9B(H9B), C7B(H7B), C8B(H8B), C10A(H10A), C4B(H4B), C4C(H4C),
 C1A(H1A), C1C(H1C), C11C(H11C), C5C(H5C), C2C(H2C), C9C(H9C)
5.b Secondary CH2 refined with riding coordinates:
 C5A(H5Aa,H5Ab), C11A(H11a,H11b), C6C(H6Ca,H6Cb), C12C(H12b,H12c), C12B(H12d,
 H12e), C6B(H6Ba,H6Bb)
;
_shelx_res_checksum              23982
_olex2_submission_special_instructions 'No special instructions were received'