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_7123918
_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_formula_moiety
'C105 H109 K2.5 N9 O79.5 Re9 Se12, C6 N6 Re6 Se8, 0.5(O)'
_chemical_formula_sum            'C111 H109 K2.5 N15 O80 Re15 Se20'
_chemical_formula_weight         7403.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-28
_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                   35.247(4)
_cell_length_b                   35.747(4)
_cell_length_c                   17.7344(17)
_cell_measurement_reflns_used    9224
_cell_measurement_temperature    200
_cell_measurement_theta_max      26.273
_cell_measurement_theta_min      2.31
_cell_volume                     22345(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.1199
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            512434
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         0.811
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.467
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1608 before and 0.0795 after correction. The Ratio of minimum to maximum transmission is 0.4614. 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    2.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             13490
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.644
_refine_diff_density_min         -5.084
_refine_diff_density_rms         0.383
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.194(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         45816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0819
_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^)+(0.0761P)^2^+1332.8652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.2308
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                31241
_reflns_number_total             45816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05136h2.cif
_cod_data_source_block           iaa444a
_cod_original_formula_sum        'C111 H109 K2.50 N15 O80 Re15 Se20'
_cod_database_code               7123918
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.657
_shelx_estimated_absorpt_t_min   0.340
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.806(18)
 0.194(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C7E) = Uanis(C8E) = Uanis(C9E) = Uanis(C10E) = Uanis(C11E) = Uanis(C12E)
= Uanis(C6E) = Uanis(C5E) = Uanis(C4E) = Uanis(C3E) = Uanis(C2E) = Uanis(C1E) =
Uanis(C48E) = Uanis(C47E) = Uanis(C46E) = Uanis(C45E) = Uanis(C44E) =
Uanis(C43E) = Uanis(C42E) = Uanis(C41E) = Uanis(C40E) = Uanis(C39E) =
Uanis(C38E) = Uanis(C37E) = Uanis(C36E) = Uanis(C35E) = Uanis(C34E) =
Uanis(C33E) = Uanis(C32E) = Uanis(C31E) = Uanis(C30E) = Uanis(C29E) =
Uanis(C28E) = Uanis(C27E) = Uanis(C26E) = Uanis(C25E) = Uanis(C24E) =
Uanis(C23E) = Uanis(C22E) = Uanis(C21E) = Uanis(C20E) = Uanis(C19E) =
Uanis(C17E) = Uanis(C18E) = Uanis(C16E) = Uanis(C15E) = Uanis(C14E) =
Uanis(C13E) = Uanis(C7F) = Uanis(C8F) = Uanis(C9F) = Uanis(C10F) = Uanis(C11F)
= Uanis(C12F) = Uanis(C6F) = Uanis(C5F) = Uanis(C4F) = Uanis(C3F) = Uanis(C2F)
= Uanis(C1F) = Uanis(C48F) = Uanis(C47F) = Uanis(C44F) = Uanis(C43F) =
Uanis(C42F) = Uanis(C41F) = Uanis(C40F) = Uanis(C39F) = Uanis(C38F) =
Uanis(C37F) = Uanis(C36F) = Uanis(C35F) = Uanis(C34F) = Uanis(C33F) =
Uanis(C32F) = Uanis(C31F) = Uanis(C30F) = Uanis(C29F) = Uanis(C28F) =
Uanis(C27F) = Uanis(C26F) = Uanis(C25F) = Uanis(C24F) = Uanis(C23F) =
Uanis(C22F) = Uanis(C21F) = Uanis(C20F) = Uanis(C19F) = Uanis(C17F) =
Uanis(C18F) = Uanis(C16F) = Uanis(C15F) = Uanis(C14F) = Uanis(C13F) =
Uanis(C46F) = Uanis(C45F)
Uanis(O26E) = Uanis(O29E) = Uanis(O25E) = Uanis(O27E) = Uanis(O28E) =
Uanis(O30E) = Uanis(O31E) = Uanis(O34E) = Uanis(O32E) = Uanis(O33E) =
Uanis(O35E) = Uanis(O1E) = Uanis(O39E) = Uanis(O36E) = Uanis(O38E) =
Uanis(O37E) = Uanis(O40E) = Uanis(O2E) = Uanis(O3E) = Uanis(O4E) = Uanis(O5E) =
Uanis(O6E) = Uanis(O9E) = Uanis(O8E) = Uanis(O7E) = Uanis(O10E) = Uanis(O11E) =
Uanis(O14E) = Uanis(O13E) = Uanis(O12E) = Uanis(O15E) = Uanis(O17E) =
Uanis(O16E) = Uanis(O19E) = Uanis(O18E) = Uanis(O20E) = Uanis(O22E) =
Uanis(O23E) = Uanis(O24E) = Uanis(O21E) = Uanis(O26F) = Uanis(O29F) =
Uanis(O25F) = Uanis(O27F) = Uanis(O28F) = Uanis(O30F) = Uanis(O31F) =
Uanis(O34F) = Uanis(O32F) = Uanis(O33F) = Uanis(O35F) = Uanis(O1F) =
Uanis(O39F) = Uanis(O36F) = Uanis(O38F) = Uanis(O37F) = Uanis(O40F) =
Uanis(O2F) = Uanis(O3F) = Uanis(O4F) = Uanis(O5F) = Uanis(O6F) = Uanis(O9F) =
Uanis(O8F) = Uanis(O7F) = Uanis(O10F) = Uanis(O11F) = Uanis(O14F) = Uanis(O13F)
= Uanis(O12F) = Uanis(O15F) = Uanis(O17F) = Uanis(O16F) = Uanis(O19F) =
Uanis(O18F) = Uanis(O20F) = Uanis(O22F) = Uanis(O23F) = Uanis(O24F) =
Uanis(O21F)
Uanis(C6) = Uanis(C13) = Uanis(C14) = Uanis(C18) = Uanis(C17) = Uanis(C15) =
Uanis(C16) = Uanis(C22) = Uanis(C21) = Uanis(C20) = Uanis(C19) = Uanis(C1) =
Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5)
Uanis(N6) = Uanis(N13) = Uanis(N14) = Uanis(N18) = Uanis(N17) = Uanis(N15) =
Uanis(N16) = Uanis(N22) = Uanis(N21) = Uanis(N20) = Uanis(N19) = Uanis(N1) =
Uanis(N2) = Uanis(N3) = Uanis(N4) = Uanis(N5)
Uanis(Re11) = Uanis(Re7)
Uiso(C9) = Uiso(N9) = Uiso(C11) = Uiso(N11) = Uiso(C10) = Uiso(N10) = Uiso(C8)
= Uiso(N8) = Uiso(C7) = Uiso(N7) = Uiso(C12) = Uiso(N12)
Uiso(C9) = Uiso(N9) = Uiso(C8) = Uiso(N8) = Uiso(C10) = Uiso(N10) = Uiso(C11) =
Uiso(N11) = Uiso(C12) = Uiso(N12) = Uiso(C7) = Uiso(N7)
Uanis(Se12) = Uanis(Se11) = Uanis(Se13) = Uanis(Se14) = Uanis(Se15) =
Uanis(Se16) = Uanis(Se10) = Uanis(Se9)
4. Others
 Fixed Sof: Re18(0.825) Re15(0.825) Re20(0.825) Re22(0.825) Se28(0.825)
 Se18(0.825) Se22(0.825) Se32(0.825) Se24(0.825) Se25(0.825) Se30(0.825)
 Se20(0.825) O36E(0.5) O1W(0.5) C15(0.825) N22(0.825) C20(0.825) N20(0.825)
 N15(0.825) C22(0.825) N18(0.825) C18(0.825) Re11(0.5) Re7(0.5) C16(0.175)
 N16(0.175) Re16(0.175) Se31(0.175) Re21(0.175) Se19(0.175) Re17(0.175)
 Se26(0.175) Se27(0.175) Se29(0.175) Re19(0.175) C21(0.175) Se17(0.175)
 C19(0.175) Se23(0.175) C17(0.175) Se21(0.175) N21(0.175) N19(0.175) N17(0.175)
 Se11(0.5) Re12(0.5) Re9(0.5) Re10(0.5) Se10(0.5) Se12(0.5) Se9(0.5) C11(0.5)
 Re8(0.5) Se14(0.5) Se15(0.5) C12(0.5) Se13(0.5) C7(0.5) Se16(0.5) C9(0.5)
 C10(0.5) N11(0.5) C8(0.5) N12(0.5) N7(0.5) N9(0.5) N10(0.5) N8(0.5)
5.a Free rotating group:
 C16(N16,Re16,Se31,Re21,Se19,Re17,Se26,Se27,Se29,Re19,C21,Se17,C19,Se23,C17,
 Se21,N21,N19,N17), C27E(C28E,C26E,O22E,C29E,O24E,C25E,O23E,C30E,O21E),
 C21E(C22E,C20E,O17E,C23E,O19E,C19E,O18E,O16E), C3E(C4E,C2E,O2E,C5E,O4E,C1E,O3E,
 C6E,O1E), C45F(C46F,C44F,O37F,C47F,O39F,C43F,O38F,C48F,O36F), C9F(C10F,C8F,O7F,
 C11F,O9F,C7F,O8F,C12F,O6F), C21F(C22F,C20F,O17F,C23F,O19F,C19F,O18F,C24F,O16F),
  Se11(Re12,Re9,Re10,Se10,Se12,Se9,C11,Re8,Se14,Se15,C12,Se13,C7,Se16,C9,C10,
 N11,C8,N12,N7,N9,N10,N8)
5.b Ternary CH refined with riding coordinates:
 C16E(H16E), C15E(H15E), C9E(H9E), C8E(H8E), C12E(H12E), C10E(H10E),
 C11E(H11E), C45E(H45E), C48E(H48E), C47E(H47E), C46E(H46E), C44E(H44E),
 C17E(H17E), C18E(H18E), C14E(H14E), C39E(H39E), C36E(H36E), C40E(H40E),
 C42E(H42E), C41E(H41E), C38E(H38E), C32E(H32E), C34E(H34E), C33E(H33E),
 C35E(H35E), C16F(H16F), C3F(H3F), C15F(H15F), C6F(H6F), C4F(H4F), C5F(H5F),
 C39F(H39F), C42F(H42F), C18F(H18F), C40F(H40F), C17F(H17F), C41F(H41F),
 C2F(H2F), C33F(H33F), C36F(H36F), C28F(H28F), C34F(H34F), C35F(H35F),
 C32F(H32F), C26F(H26F), C38F(H38F), C27F(H27F), C29F(H29F), C30F(H30F),
 C27E(H27E), C28E(H28E), C26E(H26E), C29E(H29E), C30E(H30E), C21E(H21E),
 C22E(H22E), C20E(H20E), C23E(H23E), C3E(H3E), C4E(H4E), C2E(H2E), C5E(H5E),
 C6E(H6E), C45F(H45F), C46F(H46F), C44F(H44F), C47F(H47F), C48F(H48F), C9F(H9F),
  C10F(H10F), C8F(H8F), C11F(H11F), C12F(H12F), C21F(H21F), C22F(H22F),
 C20F(H20F), C23F(H23F)
5.c Secondary CH2 refined with riding coordinates:
 C7E(H7EA,H7EB), C13E(H13C,H13D), C31E(H31C,H31D), C37E(H37C,H37D), C37F(H37A,
 H37B), C25F(H25A,H25B), C31F(H31A,H31B), C1F(H1FA,H1FB), C43E(H43C,H43D),
 C25E(H25C,H25D), C19E(H19C,H19D), C1E(H1EA,H1EB), C43F(H43A,H43B), C7F(H7FA,
 H7FB), C13F(H13A,H13B), C19F(H19A,H19B)
;
_shelx_res_checksum              75666
_shelx_fab_checksum              87082
_olex2_submission_special_instructions 'No special instructions were received'