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_7125974
_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, 2(C30)'
_chemical_formula_sum            'C100 H50 Cu10 N20'
_chemical_formula_weight         2167.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 91.966(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4531(2)
_cell_length_b                   30.8052(6)
_cell_length_c                   12.2818(2)
_cell_measurement_reflns_used    11083
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      64.7410
_cell_measurement_theta_min      4.4730
_cell_volume                     3952.53(13)
_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      300(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16424
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        65.213
_diffrn_reflns_theta_max         65.213
_diffrn_reflns_theta_min         4.469
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.399
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68410
_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    1.821
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         3379
_refine_ls_number_restraints     2358
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0503P)^2^+1.6755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3092
_reflns_number_total             3379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00532k2.cif
_cod_data_source_block           C60-Saturn-300K
_cod_depositor_comments
'Adding full bibliography for 7125968--7125975.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7125974
_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
 C28-C25 \\sim C29-C24 \\sim C31-C30 \\sim C32-C23 \\sim C33-C12 \\sim C13-C22
\\sim C17-C15 \\sim C21-C26
 \\sim C20-C27 \\sim C34-C36 \\sim C14-C37 \\sim C40-C16 \\sim C18-C41 \\sim
C39-C38
 with sigma of 0.02
 C24-C25 \\sim C23-C24 \\sim C22-C26 \\sim C22-C23 \\sim C25-C26 \\sim C28-C27
\\sim C30-C29 \\sim C31-C35
 \\sim C32-C31 \\sim C33-C34 \\sim C33-C32 \\sim C12-C14 \\sim C13-C15 \\sim
C13-C12 \\sim C17-C18 \\sim C21-
 C17 \\sim C20-C19 \\sim C20-C21 \\sim C34-C35 \\sim C36-C37 \\sim C16-C15
\\sim C16-C14 \\sim C40-C41 ~
 C19-C18 \\sim C38-C37 \\sim C39-C40
 with sigma of 0.02
 C23-C25 \\sim C33-C35 \\sim C13-C16 \\sim C21-C18 \\sim C23-C26 \\sim C22-C25
\\sim C31-C33 \\sim C32-C35
 \\sim C12-C16 \\sim C13-C14 \\sim C21-C19 \\sim C20-C18 \\sim C41-C39 \\sim
C24-C22 \\sim C24-C26 \\sim C31-
 C34 \\sim C32-C34 \\sim C12-C15 \\sim C15-C14 \\sim C17-C19 \\sim C17-C20
\\sim C36-C38
 with sigma of 0.04
 C24-C32 \\sim C24-C28 \\sim C23-C13 \\sim C23-C33 \\sim C22-C15 \\sim C26-C17
\\sim C25-C27 \\sim C25-C21
 \\sim C29-C31 \\sim C30-C35 \\sim C33-C13 \\sim C12-C34 \\sim C15-C40 \\sim
C17-C41 \\sim C21-C27 \\sim C36-
 C14 \\sim C37-C16 \\sim C37-C39 \\sim C16-C39 \\sim C24-C30 \\sim C23-C31
\\sim C23-C29 \\sim C22-C21 ~
 C26-C13 \\sim C25-C29 \\sim C30-C32 \\sim C33-C36 \\sim C33-C14 \\sim C12-C37
\\sim C13-C17 \\sim C15-C18
 \\sim C15-C21 \\sim C17-C16 \\sim C27-C19 \\sim C35-C36 \\sim C34-C37 \\sim
C16-C41 \\sim C40-C18 \\sim C22-
 C32 \\sim C22-C12 \\sim C26-C20 \\sim C26-C28 \\sim C28-C20 \\sim C32-C12
\\sim C14-C40 \\sim C14-C38 ~
 C40-C38 \\sim C41-C19
 with sigma of 0.04
3. Restrained planarity
 C24, C25, C28, C29
 with sigma of 0.1
 C22, C23, C24, C25
 with sigma of 0.1
 C23, C24, C31, C32
 with sigma of 0.1
 C23, C30, C31, C32
 with sigma of 0.1
 C21, C25, C26, C28
 with sigma of 0.1
 C31, C33, C34, C35
 with sigma of 0.1
 C31, C32, C34, C35
 with sigma of 0.1
 C12, C13, C14, C16
 with sigma of 0.1
 C12, C13, C14, C15
 with sigma of 0.1
 C17, C18, C20, C21
 with sigma of 0.1
 C17, C18, C19, C21
 with sigma of 0.1
 C14, C37, C38, C39
 with sigma of 0.1
 C16, C38, C39, C40
 with sigma of 0.1
4. Rigid bond restraints
 C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
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: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
6. Rigid body (RIGU) restrains
 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
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H11a(0.5) H11b(0.5) H11c(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)
8.a Riding coordinates:
 C11(H11a,H11b,H11c)
8.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C9(H9)
8.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C8(H8a,H8b,H8c)
;
_shelx_res_checksum              30813