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_7125972
_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, C60'
_chemical_formula_sum            'C100 H50 Cu10 N20'
_chemical_formula_weight         2167.10
_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             2019-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-26 deposited with the CCDC.	2020-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.741(2)
_cell_angle_beta                 107.985(2)
_cell_angle_gamma                91.592(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3877(2)
_cell_length_b                   12.2263(3)
_cell_length_c                   16.1951(4)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      64.8940
_cell_measurement_theta_min      4.4740
_cell_volume                     1955.07(8)
_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 (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_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      4.00  29.00   0.50    0.50    --    0.00 -77.00 -60.00   50
  2  \w    -15.00  23.00   0.50    0.50    --    0.00  19.00 -90.00   76
  3  \w    -12.00  15.00   0.50    0.50    --    0.00 -38.00   0.00   54
  4  \w     31.00  57.00   0.50    0.50    --    0.00  57.00 -60.00   52
  5  \w    -87.00 -31.00   0.50    0.50    --    0.00 -77.00 -60.00  112
  6  \w     -7.00  20.00   0.50    0.50    --    0.00  57.00 -60.00   54
  7  \w     63.00  88.00   0.50    0.50    --    0.00  19.00 -90.00   50
  8  \w    -85.00 -60.00   0.50    0.50    --    0.00 -38.00   0.00   50
  9  \w     50.00  94.00   0.50    1.39    --   77.80 -30.00-180.00   88
 10  \w     55.00 133.00   0.50    1.39    --   77.80  15.00-180.00  156
 11  \w     -7.00  24.00   0.50    1.39    --   77.80 -30.00-180.00   62
 12  \w    138.00 164.00   0.50    1.39    --   77.80  15.00-180.00   52
 13  \w     -8.00 101.00   0.50    1.39    --   77.80 -61.00-180.00  218
 14  \w     -9.00  32.00   0.50    1.39    --   77.80 -82.00 120.00   82
 15  \w    -11.00 100.00   0.50    1.39    --   77.80 -61.00  60.00  222
 16  \w     66.00  95.00   0.50    1.39    --   77.80 -82.00   0.00   58
 17  \w     16.00  42.00   0.50    1.39    --   77.80 -82.00   0.00   52
 18  \w     37.00 105.00   0.50    1.39    --   77.80 -82.00 -60.00  136
 19  \w     75.00 101.00   0.50    1.39    --   77.80 -82.00-120.00   52
 20  \w     13.00  39.00   0.50    1.39    --   77.80 -82.00-120.00   52
 21  \w     24.00 105.00   0.50    1.39    --   77.80 -82.00-180.00  162
 22  \w     74.00 100.00   0.50    1.39    --   77.80 -82.00 120.00   52
 23  \w     17.00  98.00   0.50    1.39    --   77.80 -61.00 -60.00  162
 24  \w    -12.00 104.00   0.50    1.39    --   77.80 -82.00  60.00  232
 25  \w     -4.00  88.00   0.50    1.39    --   77.80 -15.00-120.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1044205000
_diffrn_orient_matrix_UB_12      0.0709204000
_diffrn_orient_matrix_UB_13      -0.0271292000
_diffrn_orient_matrix_UB_21      -0.0728779000
_diffrn_orient_matrix_UB_22      0.1038504000
_diffrn_orient_matrix_UB_23      0.0129158000
_diffrn_orient_matrix_UB_31      0.0901391000
_diffrn_orient_matrix_UB_32      0.0090966000
_diffrn_orient_matrix_UB_33      0.0954186000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18536
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        65.382
_diffrn_reflns_theta_max         65.382
_diffrn_reflns_theta_min         3.617
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74691
_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    1.841
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.529
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         6524
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+7.8978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2228
_refine_ls_wR_factor_ref         0.2290
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5544
_reflns_number_total             6524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00532k2.cif
_cod_data_source_block           c60-saturn-200k
_cod_depositor_comments
'Adding full bibliography for 7125968--7125975.cif.'
_cod_database_code               7125972
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Cu'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C28, C21, C22, C25, C40, C23, C48, C24, C26, C50, C30, C47, C49, C27, C29,
 C39, C46, C41, C34, C38, C45, C42, C31, C33, C37, C44, C43, C32, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.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)
4.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              62788
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.453
_oxdiff_exptl_absorpt_empirical_full_min 0.655