Ring size matters: supramolecular isomerism in self-assembled redox-active tetra- and hexaruthenium macrocycles.
Fink, Daniel; Orth, Nicole; Linseis, Michael; Ivanović-Burmazović, Ivana; Winter, Rainer F.; Chemical communications (Cambridge, England) 56 (2020) 1062–1065; doi:10.1039/c9cc09307a

data_7125653
_publ_section_title
;
 Ring size matters: supramolecular isomerism in self-assembled
 redox-active tetra- and hexaruthenium macrocycles.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1062
_journal_page_last               1065
_journal_paper_doi               10.1039/c9cc09307a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C104 H184 O14 P8 Ru4 S2, 5(C6 H6)'
_chemical_formula_sum            'C134 H214 O14 P8 Ru4 S2'
_chemical_formula_weight         2765.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2019-10-27 deposited with the CCDC.	2019-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                102.732(6)
_cell_angle_beta                 98.198(6)
_cell_angle_gamma                101.465(6)
_cell_formula_units_Z            1
_cell_length_a                   11.9389(9)
_cell_length_b                   17.3830(15)
_cell_length_c                   18.6230(15)
_cell_measurement_reflns_used    22812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      1.80
_cell_volume                     3623.7(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1519
_diffrn_reflns_av_unetI/netI     0.1730
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52347
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.858
_diffrn_reflns_theta_min         1.774
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.9553
_exptl_absorpt_correction_T_min  0.8579
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         15420
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0094P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8546
_reflns_number_total             15420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09307a2.cif
_cod_data_source_block           pdf33
_cod_depositor_comments
'Adding full bibliography for 7125652--7125653.cif.'
_cod_database_code               7125653
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups
2. Restrained distances
 C57-C58 = C58-C53 = C53-C54 = C54-C55 = C55-C56 = C56-C57
 1.39 with sigma of 0.005
 C59-C60 = C60-C61
 1.39 with sigma of 0.005
3.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C23(H23), C29(H29), C26(H26), C32(H32), C41(H41),
 C35(H35), C38(H38), C44(H44), C47(H47), C50(H50)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C11(H11), C12(H12), C5(H5), C6(H6), C8(H8), C56(H56),
 C57(H57), C58(H58), C53(H53), C54(H54), C55(H55), C61(H61), C60(H60), C59(H59),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C37(H37A,H37B,
 H37C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              8147
_olex2_submission_special_instructions 'No special instructions were received'