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_7125969
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-26 deposited with the CCDC.	2020-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                96.008(2)
_cell_angle_beta                 108.765(2)
_cell_angle_gamma                90.917(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8822(2)
_cell_length_b                   12.4297(2)
_cell_length_c                   16.2388(3)
_cell_measurement_reflns_used    13593
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      64.2400
_cell_measurement_theta_min      2.8730
_cell_volume                     2065.44(7)
_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_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0173
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18849
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        64.577
_diffrn_reflns_theta_max         64.577
_diffrn_reflns_theta_min         2.894
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.296
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.77730
_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    1.839
_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         0.387
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         6769
_refine_ls_number_restraints     7523
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0473P)^2^+1.2691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6284
_reflns_number_total             6769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00532k2.cif
_cod_data_source_block           C70-Saturn-250K
_cod_depositor_comments
'Adding full bibliography for 7125968--7125975.cif.'
_cod_database_code               7125969
_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 C8-C23 \\sim C44-C43 \\sim C58-C39
\\sim C18-C19 \\sim C33-C53
 \\sim C11-C10 \\sim C16-C15 \\sim C55-C54 \\sim C35-C34 \\sim C37-C38 \\sim
C45-C46 \\sim C56-C57 \\sim C26-C9
 \\sim C17-C36 \\sim C28-C27 \\sim C47-C48 \\sim C25-C24
 with sigma of 0.02
 C42-C22 \\sim C40-C20 \\sim C2-C7 \\sim C4-C5 \\sim C32-C14 \\sim C30-C12
\\sim C70-C59 \\sim C62-C61 ~
 C50-C65 \\sim C52-C67
 with sigma of 0.02
 C69-C70 \\sim C32-C33 \\sim C30-C29 \\sim C14-C15 \\sim C12-C11 \\sim C63-C62
\\sim C68-C67 \\sim C8-C7 ~
 C59-C58 \\sim C61-C44 \\sim C18-C5 \\sim C53-C52 \\sim C49-C50 \\sim C42-C43
\\sim C22-C23 \\sim C40-C39 ~
 C20-C19 \\sim C10-C2 \\sim C4-C16 \\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 C1-C66 \\sim C31-C51 \\sim C13-C3 \\sim C21-C6
 with sigma of 0.02
 C22-C21 \\sim C32-C31 \\sim C31-C30 \\sim C14-C13 \\sim C12-C13 \\sim C70-C1
\\sim C62-C1 \\sim C59-C60 ~
 C60-C61 \\sim C21-C20 \\sim C6-C7 \\sim C6-C5 \\sim C51-C52 \\sim C51-C50
\\sim C65-C66 \\sim C66-C67 ~
 C42-C41 \\sim C41-C40 \\sim C2-C3 \\sim C3-C4
 with sigma of 0.02
 C29-C28 \\sim C45-C44 \\sim C8-C9 \\sim C58-C57 \\sim C34-C15 \\sim C34-C33
\\sim C18-C17 \\sim C39-C38 ~
 C28-C11 \\sim C43-C24 \\sim C69-C57 \\sim C45-C63 \\sim C68-C54 \\sim C54-C53
\\sim C9-C10 \\sim C17-C16 ~
 C23-C24 \\sim C19-C38 \\sim C49-C48 \\sim C48-C64
 with sigma of 0.02
 C11-C29 \\sim C10-C8 \\sim C18-C16 \\sim C68-C53 \\sim C33-C15 \\sim C49-C64
\\sim C63-C44 \\sim C43-C23
 \\sim C19-C39 \\sim C58-C69 \\sim C11-C30 \\sim C10-C7 \\sim C2-C8 \\sim
C4-C18 \\sim C49-C65 \\sim C29-C12 ~
 C32-C15 \\sim C14-C33 \\sim C63-C61 \\sim C67-C53 \\sim C52-C68 \\sim C43-C22
\\sim C44-C62 \\sim C59-C69
 \\sim C70-C58 \\sim C23-C42 \\sim C20-C39 \\sim C40-C19 \\sim C5-C16 \\sim
C64-C50
 with sigma of 0.04
 C2-C4 \\sim C30-C32 \\sim C12-C14 \\sim C65-C67 \\sim C50-C52 \\sim C61-C59
\\sim C62-C70 \\sim C22-C20 ~
 C42-C40 \\sim C7-C5
 with sigma of 0.04
 C64-C62 \\sim C10-C12 \\sim C49-C30 \\sim C29-C50 \\sim C32-C53 \\sim C14-C16
\\sim C63-C65 \\sim C67-C69
 \\sim C52-C33 \\sim C43-C61 \\sim C59-C39 \\sim C70-C68 \\sim C23-C7 \\sim
C5-C19 \\sim C11-C2 \\sim C4-C15 ~
 C44-C42 \\sim C8-C22 \\sim C20-C18 \\sim C40-C58 \\sim C28-C10 \\sim C9-C23
\\sim C19-C17 \\sim C34-C16 ~
 C28-C49 \\sim C11-C9 \\sim C48-C29 \\sim C48-C63 \\sim C45-C64 \\sim C45-C43
\\sim C24-C8 \\sim C24-C44 ~
 C38-C58 \\sim C38-C18 \\sim C57-C39 \\sim C54-C69 \\sim C54-C33 \\sim C34-C53
\\sim C17-C15 \\sim C57-C68
 \\sim C28-C47 \\sim C28-C26 \\sim C27-C48 \\sim C48-C46 \\sim C47-C45 \\sim
C45-C25 \\sim C46-C24 \\sim C24-
 C26 \\sim C25-C9 \\sim C38-C36 \\sim C38-C56 \\sim C37-C17 \\sim C37-C57 \\sim
C57-C55 \\sim C56-C54 \\sim C54-
 C35 \\sim C55-C34 \\sim C34-C36 \\sim C27-C9 \\sim C35-C17 \\sim C11-C27 \\sim
C27-C29 \\sim C10-C26 \\sim C49-
 C47 \\sim C63-C46 \\sim C46-C44 \\sim C43-C25 \\sim C25-C23 \\sim C8-C26 \\sim
C19-C37 \\sim C18-C36 \\sim C37-
 C39 \\sim C58-C56 \\sim C56-C69 \\sim C55-C53 \\sim C33-C35 \\sim C35-C15
\\sim C16-C36 \\sim C47-C64 ~
 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 C9-C7 \\sim C5-C17 \\sim C28-C12 \\sim
C28-C30 \\sim C2-C9 \\sim C4-C17 ~
 C48-C50 \\sim C48-C65 \\sim C32-C34 \\sim C14-C34 \\sim C45-C62 \\sim C45-C61
\\sim C67-C54 \\sim C52-C54
 \\sim C24-C22 \\sim C24-C42 \\sim C59-C57 \\sim C70-C57 \\sim C20-C38 \\sim
C40-C38
 with sigma of 0.04
 C3-C12 \\sim C3-C14 \\sim C30-C51 \\sim C31-C52 \\sim C31-C50 \\sim C32-C51
\\sim C65-C1 \\sim C66-C70 ~
 C66-C62 \\sim C67-C1 \\sim C61-C41 \\sim C59-C41 \\sim C22-C6 \\sim C20-C6
\\sim C2-C13 \\sim C4-C13 \\sim C60-
 C40 \\sim C60-C42 \\sim C21-C7 \\sim C21-C5 \\sim C2-C6 \\sim C4-C6 \\sim
C31-C14 \\sim C31-C12 \\sim C65-C51
 \\sim C67-C51 \\sim C21-C40 \\sim C21-C42 \\sim C3-C7 \\sim C3-C5 \\sim
C30-C13 \\sim C32-C13 \\sim C66-C50 ~
 C66-C52 \\sim C61-C1 \\sim C60-C70 \\sim C60-C62 \\sim C59-C1 \\sim C22-C41
\\sim C20-C41
 with sigma of 0.04
 C11-C13 \\sim C10-C3 \\sim C3-C16 \\sim C49-C51 \\sim C29-C31 \\sim C31-C33
\\sim C13-C15 \\sim C63-C1 ~
 C64-C66 \\sim C66-C68 \\sim C51-C53 \\sim C43-C41 \\sim C44-C60 \\sim C60-C58
\\sim C1-C69 \\sim C8-C6 ~
 C23-C21 \\sim C21-C19 \\sim C41-C39 \\sim C6-C18
 with sigma of 0.04
3. Restrained planarity
 C2, C3, C12, C13
 with sigma of 0.1
 C2, C8, C9, C10
 with sigma of 0.1
 C7, C8, C9, C10
 with sigma of 0.1
 C11, C12, C28, C29
 with sigma of 0.1
 C11, C28, C29, C30
 with sigma of 0.1
 C12, C13, C14, C30
 with sigma of 0.1
 C14, C15, C32, C34
 with sigma of 0.1
 C14, C15, C33, C34
 with sigma of 0.1
 C15, C16, C17, C34
 with sigma of 0.1
 C5, C16, C17, C18
 with sigma of 0.1
 C16, C17, C35, C36
 with sigma of 0.1
 C4, C5, C17, C18
 with sigma of 0.1
 C17, C18, C19, C38
 with sigma of 0.1
 C19, C36, C37, C38
 with sigma of 0.1
 C20, C21, C40, C41
 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
 C8, C9, C25, C26
 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
 C1, C62, C63, C64
 with sigma of 0.1
 C1, C64, C65, C66
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim 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: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, 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
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1(0.5) C2(0.5) C3(0.5) C4(0.5) C5(0.5) C6(0.5) C7(0.5) C8(0.5)
 C9(0.5) C10(0.5) C11(0.5) C12(0.5) C13(0.5) C14(0.5) C15(0.5) C16(0.5)
 C17(0.5) C18(0.5) C19(0.5) C20(0.5) 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)
7.a Aromatic/amide H refined with riding coordinates:
 C73(H73), C74(H74), C77(H77), C78(H78), C81(H81), C82(H82), C83(H83),
 C84(H84), C87(H87), C88(H88)
7.b Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C75(H75A,H75B,H75C), C79(H79A,H79B,H79C), C85(H85A,H85B,
 H85C), C90(H90A,H90B,H90C)
;