Coordination disk-type nano-Saturn complexes.
Zhan, Shun-Ze; Li, Jing-Hong; Zhang, Guo-Hui; Li, Ming-De; Sun, Shanshan; Zheng, Ji; Ning, Guo-Hong; Li, Mian; Kuang, Dai-Bin; Wang, Xu-Dong; Li, Dan; Chemical communications (Cambridge, England) 56 (2020) 3325–3328; doi:10.1039/d0cc00532k

data_7125971
_publ_section_title
;
 Coordination disk-type nano-Saturn complexes.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3325
_journal_page_last               3328
_journal_paper_doi               10.1039/d0cc00532k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C40 H50 Cu10 N20, 0.5(C140)'
_chemical_formula_sum            'C110 H50 Cu10 N20'
_chemical_formula_weight         2287.20
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-22
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.11 svn.r3635 for OlexSys, GUI svn.r5848)
;
_audit_update_record
;
2019-07-26 deposited with the CCDC.	2020-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                95.7000(10)
_cell_angle_beta                 108.7480(10)
_cell_angle_gamma                91.3920(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8776(2)
_cell_length_b                   12.45240(10)
_cell_length_c                   16.2822(2)
_cell_measurement_reflns_used    30810
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      64.9660
_cell_measurement_theta_min      3.5330
_cell_volume                     2074.41(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40820
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        65.215
_diffrn_reflns_theta_max         65.215
_diffrn_reflns_theta_min         2.885
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.051
_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     951
_refine_ls_number_reflns         6968
_refine_ls_number_restraints     7523
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0490P)^2^+1.1599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6853
_reflns_number_total             6968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00532k2.cif
_cod_data_source_block           C70-Saturn-300K
_cod_depositor_comments
'Adding full bibliography for 7125968--7125975.cif.'
_cod_database_code               7125971
_shelx_shelxl_version_number     2018/3
_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
 C63-C64 \\sim C69-C68 \\sim C29-C49 \\sim C78-C23 \\sim C44-C43 \\sim C58-C39
\\sim C88-C89 \\sim C33-C53
 \\sim C81-C80 \\sim C86-C85 \\sim C55-C54 \\sim C35-C34 \\sim C37-C38 \\sim
C45-C46 \\sim C56-C57 \\sim C26-
 C79 \\sim C87-C36 \\sim C28-C27 \\sim C47-C48 \\sim C25-C24
 with sigma of 0.02
 C42-C22 \\sim C40-C90 \\sim C72-C77 \\sim C74-C75 \\sim C32-C84 \\sim C30-C82
\\sim C70-C59 \\sim C62-C61
 \\sim C50-C65 \\sim C52-C67
 with sigma of 0.02
 C69-C70 \\sim C32-C33 \\sim C30-C29 \\sim C84-C85 \\sim C82-C81 \\sim C63-C62
\\sim C68-C67 \\sim C78-C77
 \\sim C59-C58 \\sim C61-C44 \\sim C88-C75 \\sim C53-C52 \\sim C49-C50 \\sim
C42-C43 \\sim C22-C23 \\sim C40-
 C39 \\sim C90-C89 \\sim C80-C72 \\sim C74-C86 \\sim C64-C65
 with sigma of 0.02
 C55-C56 \\sim C55-C35 \\sim C46-C47 \\sim C27-C47 \\sim C35-C36 \\sim C37-C36
\\sim C37-C56 \\sim C46-C25
 \\sim C26-C27 \\sim C26-C25
 with sigma of 0.02
 C41-C60 \\sim C71-C66 \\sim C31-C51 \\sim C83-C73 \\sim C21-C76
 with sigma of 0.02
 C22-C21 \\sim C32-C31 \\sim C31-C30 \\sim C84-C83 \\sim C82-C83 \\sim C70-C71
\\sim C62-C71 \\sim C59-C60
 \\sim C60-C61 \\sim C21-C90 \\sim C76-C77 \\sim C76-C75 \\sim C51-C52 \\sim
C51-C50 \\sim C65-C66 \\sim C66-
 C67 \\sim C42-C41 \\sim C41-C40 \\sim C72-C73 \\sim C73-C74
 with sigma of 0.02
 C29-C28 \\sim C45-C44 \\sim C78-C79 \\sim C58-C57 \\sim C34-C85 \\sim C34-C33
\\sim C88-C87 \\sim C39-C38
 \\sim C28-C81 \\sim C43-C24 \\sim C69-C57 \\sim C45-C63 \\sim C68-C54 \\sim
C54-C53 \\sim C79-C80 \\sim C87-
 C86 \\sim C23-C24 \\sim C89-C38 \\sim C49-C48 \\sim C48-C64
 with sigma of 0.02
 C81-C29 \\sim C80-C78 \\sim C88-C86 \\sim C68-C53 \\sim C33-C85 \\sim C49-C64
\\sim C63-C44 \\sim C43-C23
 \\sim C89-C39 \\sim C58-C69 \\sim C81-C30 \\sim C80-C77 \\sim C72-C78 \\sim
C74-C88 \\sim C49-C65 \\sim C29-
 C82 \\sim C32-C85 \\sim C84-C33 \\sim C63-C61 \\sim C67-C53 \\sim C52-C68
\\sim C43-C22 \\sim C44-C62 ~
 C59-C69 \\sim C70-C58 \\sim C23-C42 \\sim C90-C39 \\sim C40-C89 \\sim C75-C86
\\sim C64-C50
 with sigma of 0.04
 C72-C74 \\sim C30-C32 \\sim C82-C84 \\sim C65-C67 \\sim C50-C52 \\sim C61-C59
\\sim C62-C70 \\sim C22-C90
 \\sim C42-C40 \\sim C77-C75
 with sigma of 0.04
 C64-C62 \\sim C80-C82 \\sim C49-C30 \\sim C29-C50 \\sim C32-C53 \\sim C84-C86
\\sim C63-C65 \\sim C67-C69
 \\sim C52-C33 \\sim C43-C61 \\sim C59-C39 \\sim C70-C68 \\sim C23-C77 \\sim
C75-C89 \\sim C81-C72 \\sim C74-
 C85 \\sim C44-C42 \\sim C78-C22 \\sim C90-C88 \\sim C40-C58 \\sim C28-C80
\\sim C79-C23 \\sim C89-C87 ~
 C34-C86 \\sim C28-C49 \\sim C81-C79 \\sim C48-C29 \\sim C48-C63 \\sim C45-C64
\\sim C45-C43 \\sim C24-C78
 \\sim C24-C44 \\sim C38-C58 \\sim C38-C88 \\sim C57-C39 \\sim C54-C69 \\sim
C54-C33 \\sim C34-C53 \\sim C87-
 C85 \\sim C57-C68 \\sim C28-C47 \\sim C28-C26 \\sim C27-C48 \\sim C48-C46
\\sim C47-C45 \\sim C45-C25 ~
 C46-C24 \\sim C24-C26 \\sim C25-C79 \\sim C38-C36 \\sim C38-C56 \\sim C37-C87
\\sim C37-C57 \\sim C57-C55
 \\sim C56-C54 \\sim C54-C35 \\sim C55-C34 \\sim C34-C36 \\sim C27-C79 \\sim
C35-C87 \\sim C81-C27 \\sim C27-
 C29 \\sim C80-C26 \\sim C49-C47 \\sim C63-C46 \\sim C46-C44 \\sim C43-C25
\\sim C25-C23 \\sim C78-C26 ~
 C89-C37 \\sim C88-C36 \\sim C37-C39 \\sim C58-C56 \\sim C56-C69 \\sim C55-C53
\\sim C33-C35 \\sim C35-C85
 \\sim C86-C36 \\sim C47-C64 \\sim C68-C55
 with sigma of 0.04
 C47-C26 \\sim C47-C25 \\sim C37-C55 \\sim C55-C36 \\sim C27-C46 \\sim C27-C25
\\sim C46-C26 \\sim C37-C35
 \\sim C56-C36 \\sim C56-C35 \\sim C79-C77 \\sim C75-C87 \\sim C28-C82 \\sim
C28-C30 \\sim C72-C79 \\sim C74-
 C87 \\sim C48-C50 \\sim C48-C65 \\sim C32-C34 \\sim C84-C34 \\sim C45-C62
\\sim C45-C61 \\sim C67-C54 ~
 C52-C54 \\sim C24-C22 \\sim C24-C42 \\sim C59-C57 \\sim C70-C57 \\sim C90-C38
\\sim C40-C38
 with sigma of 0.04
 C73-C82 \\sim C73-C84 \\sim C30-C51 \\sim C31-C52 \\sim C31-C50 \\sim C32-C51
\\sim C65-C71 \\sim C66-C70
 \\sim C66-C62 \\sim C67-C71 \\sim C61-C41 \\sim C59-C41 \\sim C22-C76 \\sim
C90-C76 \\sim C72-C83 \\sim C74-
 C83 \\sim C60-C40 \\sim C60-C42 \\sim C21-C77 \\sim C21-C75 \\sim C72-C76
\\sim C74-C76 \\sim C31-C84 ~
 C31-C82 \\sim C65-C51 \\sim C67-C51 \\sim C21-C40 \\sim C21-C42 \\sim C73-C77
\\sim C73-C75 \\sim C30-C83
 \\sim C32-C83 \\sim C66-C50 \\sim C66-C52 \\sim C61-C71 \\sim C60-C70 \\sim
C60-C62 \\sim C59-C71 \\sim C22-
 C41 \\sim C90-C41
 with sigma of 0.04
 C81-C83 \\sim C80-C73 \\sim C73-C86 \\sim C49-C51 \\sim C29-C31 \\sim C31-C33
\\sim C83-C85 \\sim C63-C71
 \\sim C64-C66 \\sim C66-C68 \\sim C51-C53 \\sim C43-C41 \\sim C44-C60 \\sim
C60-C58 \\sim C71-C69 \\sim C78-
 C76 \\sim C23-C21 \\sim C21-C89 \\sim C41-C39 \\sim C76-C88
 with sigma of 0.04
3. Restrained planarity
 C72, C73, C82, C83
 with sigma of 0.1
 C72, C78, C79, C80
 with sigma of 0.1
 C77, C78, C79, C80
 with sigma of 0.1
 C28, C29, C81, C82
 with sigma of 0.1
 C28, C29, C30, C81
 with sigma of 0.1
 C30, C82, C83, C84
 with sigma of 0.1
 C32, C34, C84, C85
 with sigma of 0.1
 C33, C34, C84, C85
 with sigma of 0.1
 C34, C85, C86, C87
 with sigma of 0.1
 C75, C86, C87, C88
 with sigma of 0.1
 C35, C36, C86, C87
 with sigma of 0.1
 C74, C75, C87, C88
 with sigma of 0.1
 C38, C87, C88, C89
 with sigma of 0.1
 C36, C37, C38, C89
 with sigma of 0.1
 C21, C40, C41, C90
 with sigma of 0.1
 C22, C23, C42, C43
 with sigma of 0.1
 C23, C24, C25, C26
 with sigma of 0.1
 C25, C27, C46, C47
 with sigma of 0.1
 C25, C26, C46, C47
 with sigma of 0.1
 C25, C26, C78, C79
 with sigma of 0.1
 C29, C30, C31, C49
 with sigma of 0.1
 C29, C30, C31, C51
 with sigma of 0.1
 C30, C31, C50, C51
 with sigma of 0.1
 C33, C34, C53, C54
 with sigma of 0.1
 C33, C34, C35, C55
 with sigma of 0.1
 C37, C38, C56, C57
 with sigma of 0.1
 C41, C42, C43, C60
 with sigma of 0.1
 C41, C42, C43, C44
 with sigma of 0.1
 C42, C43, C44, C61
 with sigma of 0.1
 C44, C45, C61, C62
 with sigma of 0.1
 C44, C61, C62, C63
 with sigma of 0.1
 C45, C48, C63, C64
 with sigma of 0.1
 C46, C47, C48, C64
 with sigma of 0.1
 C47, C48, C63, C64
 with sigma of 0.1
 C48, C50, C64, C65
 with sigma of 0.1
 C49, C50, C64, C65
 with sigma of 0.1
 C50, C51, C52, C65
 with sigma of 0.1
 C52, C53, C54, C67
 with sigma of 0.1
 C52, C53, C54, C68
 with sigma of 0.1
 C57, C59, C69, C70
 with sigma of 0.1
 C58, C59, C69, C70
 with sigma of 0.1
 C62, C63, C64, C71
 with sigma of 0.1
 C64, C65, C66, C71
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim
C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim
C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim
C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35,
 C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49, C50, C51,
  C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64, C65, C66,
 C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79, C80, C81, C82,
  C83, C84, C85, C86, C87, C88, C89, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C21(0.5) C22(0.5) C23(0.5) C24(0.5) C25(0.5) C26(0.5) C27(0.5)
 C28(0.5) C29(0.5) C30(0.5) C31(0.5) C32(0.5) C33(0.5) C34(0.5) C35(0.5)
 C36(0.5) C37(0.5) C38(0.5) C39(0.5) C40(0.5) C41(0.5) C42(0.5) C43(0.5)
 C44(0.5) C45(0.5) C46(0.5) C47(0.5) C48(0.5) C49(0.5) C50(0.5) C51(0.5)
 C52(0.5) C53(0.5) C54(0.5) C55(0.5) C56(0.5) C57(0.5) C58(0.5) C59(0.5)
 C60(0.5) C61(0.5) C62(0.5) C63(0.5) C64(0.5) C65(0.5) C66(0.5) C67(0.5)
 C68(0.5) C69(0.5) C70(0.5) C71(0.5) C72(0.5) C73(0.5) C74(0.5) C75(0.5)
 C76(0.5) C77(0.5) C78(0.5) C79(0.5) C80(0.5) C81(0.5) C82(0.5) C83(0.5)
 C84(0.5) C85(0.5) C86(0.5) C87(0.5) C88(0.5) C89(0.5) C90(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C9(H9), C10(H10), C13(H13), C14(H14),
 C17(H17), C18(H18)
7.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C8(H8a,H8b,H8c), C12(H12a,H12b,H12c), C16(H16a,H16b,H16c),
 C20(H20a,H20b,H20c)
;
_shelx_res_checksum              30884
_olex2_submission_special_instructions 'No special instructions were received'