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_7125652
_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         'C156 H276 O21 P12 Ru6 S3, 6(C6 H6)'
_chemical_formula_sum            'C192 H312 O21 P12 Ru6 S3'
_chemical_formula_weight         4030.64
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-27 deposited with the CCDC.	2019-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                63.0890(10)
_cell_angle_beta                 83.8960(10)
_cell_angle_gamma                71.9420(10)
_cell_formula_units_Z            2
_cell_length_a                   23.3486(4)
_cell_length_b                   24.9671(5)
_cell_length_c                   25.2132(5)
_cell_measurement_reflns_used    42837
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      1.66
_cell_volume                     12450.7(4)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_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, 2015)'
_diffrn_ambient_temperature      100(3)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
 204 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0942
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            92182
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.250
_diffrn_reflns_theta_min         2.290
_diffrn_source
'Sealed Mo X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.9097
_exptl_absorpt_correction_T_min  0.8320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.865
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2121
_refine_ls_number_reflns         49773
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0848
_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^)+(0.1227P)^2^+12.8469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27832
_reflns_number_total             49773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09307a2.cif
_cod_data_source_block           dfbw26-3
_cod_depositor_comments
'Adding full bibliography for 7125652--7125653.cif.'
_cod_database_code               7125652
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H10r-H11a
 -2.4 with sigma of 0.02
 H10p-H11a
 -2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C76) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C105) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C186, C185, C184, C183, C182, C181
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C189, C190, C191, C192, C187, C188
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C164, C165, C166, C167, C168, C163
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C188, C189, C190, C191, C192, C187
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C184, C183, C182, C181, C186, C185
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C56, C55, C57
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C93, C91, C92
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C66, C64, C65
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C105, C103, C104
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C99, C97, C98
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C86, C85, C87
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C81, C79, C80
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Ternary CH refined with riding coordinates:
 C151(H151), C148(H148), C142(H142), C154(H154), C130(H130), C124(H124),
 C70(H70), C133(H133), C94(H94), C136(H136), C109(H109), C73(H73), C97(H97),
 C121(H121), C127(H127), C67(H67), C82(H82), C100(H100), C88(H88), C64(H64),
 C106(H106), C112(H112), C49(H49), C85(H85), C91(H91), C58(H58), C52(H52),
 C79(H79), C115(H115), C55(H55), C139(H139), C145(H145), C61(H61), C118(H118),
 C76(H76), C103(H103)
5.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C27(H27), C24(H24), C23(H23), C21(H21), C20(H20), C18(H18),
 C17(H17), C40(H40), C39(H39), C16(H16), C15(H15), C13(H13), C12(H12), C10(H10),
  C9(H9), C34(H34), C33(H33), C8(H8), C7(H7), C5(H5), C4(H4), C2(H2), C1(H1),
 C168(H168), C163(H163), C164(H164), C165(H165), C166(H166), C167(H167),
 C181(H181), C182(H182), C183(H183), C184(H184), C185(H185), C186(H186),
 C172(H172), C171(H171), C170(H170), C169(H169), C174(H174), C173(H173),
 C190(H190), C189(H189), C188(H188), C187(H187), C192(H192), C191(H191),
 C158(H158), C159(H159), C160(H160), C161(H161), C162(H162), C157(H157),
 C175(H175), C176(H176), C177(H177), C178(H178), C179(H179), C180(H180)
5.c Fitted hexagon refined as free rotating group:
 C168(C163,C164,C165,C166,C167), C181(C182,C183,C184,C185,C186), C172(C171,
 C170,C169,C174,C173), C190(C189,C188,C187,C192,C191), C175(C176,C177,C178,C179,
 C180)
5.d Idealised Me refined as rotating group:
 C141(H14a,H14b,H14c), C143(H14d,H14e,H14f), C144(H14g,H14h,H14i), C156(H15a,
 H15b,H15c), C155(H15d,H15e,H15f), C72(H72a,H72b,H72c), C147(H14j,H14k,H14l),
 C126(H12c,H12a,H12b), C83(H83a,H83b,H83c), C131(H13a,H13b,H13c), C123(H12d,
 H12e,H12f), C149(H14m,H14n,H14o), C152(H15g,H15h,H15i), C128(H12g,H12h,H12i),
 C132(H13d,H13e,H13f), C122(H12j,H12k,H12l), C135(H13g,H13h,H13i), C95(H95a,
 H95b,H95c), C110(H11a,H11b,H11c), C146(H14p,H14q,H14r), C71(H71a,H71b,H71c),
 C69(H69a,H69b,H69c), C111(H11d,H11e,H11f), C114(H11g,H11h,H11i), C101(H10a,
 H10b,H10c), C98(H98a,H98b,H98c), C63(H63a,H63b,H63c), C86(H86a,H86b,H86c),
 C90(H90a,H90b,H90c), C99(H99a,H99b,H99c), C108(H10d,H10e,H10f), C134(H13j,H13k,
 H13l), C107(H10g,H10h,H10i), C96(H96a,H96b,H96c), C59(H59a,H59b,H59c),
 C56(H56a,H56b,H56c), C93(H93a,H93b,H93c), C87(H87a,H87b,H87c), C54(H54a,H54b,
 H54c), C53(H53a,H53b,H53c), C51(H51a,H51b,H51c), C81(H81a,H81b,H81c),
 C120(H12m,H12n,H12o), C116(H11j,H11k,H11l), C117(H11m,H11n,H11o), C57(H57a,
 H57b,H57c), C50(H50a,H50b,H50c), C153(H15j,H15k,H15l), C150(H15m,H15n,H15o),
 C140(H14s,H14t,H14u), C75(H75a,H75b,H75c), C125(H12p,H12q,H12r), C129(H12s,
 H12t,H12u), C137(H13m,H13n,H13o), C138(H13p,H13q,H13r), C74(H74a,H74b,H74c),
 C92(H92a,H92b,H92c), C68(H68a,H68b,H68c), C102(H10j,H10k,H10l), C62(H62a,H62b,
 H62c), C89(H89a,H89b,H89c), C119(H11p,H11q,H11r), C60(H60a,H60b,H60c),
 C66(H66a,H66b,H66c), C84(H84a,H84b,H84c), C65(H65a,H65b,H65c), C80(H80a,H80b,
 H80c), C113(H11s,H11t,H11u), C78(H78a,H78b,H78c), C77(H77a,H77b,H77c),
 C105(H10m,H10n,H10o), C104(H10p,H10q,H10r)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35315
_shelx_fab_checksum              2631
_olex2_submission_special_instructions 'No special instructions were received'