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_7125970
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-24
_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
_cell_angle_beta                 91.742(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3986(3)
_cell_length_b                   30.8174(8)
_cell_length_c                   12.2534(3)
_cell_measurement_reflns_used    6934
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      64.7710
_cell_measurement_theta_min      4.4400
_cell_volume                     3924.88(18)
_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      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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    -17.00  18.00   0.50    0.50    --    0.00  38.00 -60.00   70
  2  \w     55.00  88.00   0.50    0.50    --    0.00  38.00 -60.00   66
  3  \w     -7.00  18.00   0.50    0.50    --    0.00 -19.00  30.00   50
  4  \w    -87.00 -62.00   0.50    0.50    --    0.00 -19.00  30.00   50
  5  \w     54.00 162.00   0.50    1.37    --   77.20  77.00   0.00  216
  6  \w     58.00 167.00   0.50    1.37    --   77.20  45.00 -30.00  218
  7  \w      9.00 107.00   0.50    1.37    --   77.20 -77.00  90.00  196
  8  \w     54.00 167.00   0.50    1.37    --   77.20  61.00-120.00  226
  9  \w     37.00 101.00   0.50    1.37    --   77.20 -61.00  90.00  128
 10  \w    123.00 149.00   0.50    1.37    --   77.20  30.00 120.00   52
 11  \w     22.00  48.00   0.50    1.37    --   77.20 -82.00-150.00   52
;
_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      -0.0072676000
_diffrn_orient_matrix_UB_12      -0.0442580000
_diffrn_orient_matrix_UB_13      -0.0585186000
_diffrn_orient_matrix_UB_21      0.0880072000
_diffrn_orient_matrix_UB_22      0.0173290000
_diffrn_orient_matrix_UB_23      -0.0889799000
_diffrn_orient_matrix_UB_31      0.1189302000
_diffrn_orient_matrix_UB_32      -0.0155255000
_diffrn_orient_matrix_UB_33      0.0670145000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0233
_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       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9946
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        65.225
_diffrn_reflns_theta_max         65.225
_diffrn_reflns_theta_min         3.609
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59711
_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_colour_primary    black
_exptl_crystal_density_diffrn    1.834
_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         1.024
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         3338
_refine_ls_number_restraints     2358
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0830P)^2^+4.1312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3031
_reflns_number_total             3338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00532k2.cif
_cod_data_source_block           C60-Saturn-250K
_cod_depositor_comments
'Adding full bibliography for 7125968--7125975.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7125970
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Cu'
_reflns_odcompleteness_completeness 99.81
_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. Restrained distances
 C34-C33 \\sim C36-C35 \\sim C38-C37 \\sim C40-C39 \\sim C43-C42 \\sim C45-C46
\\sim C47-C59 \\sim C48-C49
 \\sim C52-C51 \\sim C53-C61 \\sim C55-C54 \\sim C56-C57 \\sim C58-C44 \\sim
C60-C50
 with sigma of 0.02
 C32-C49 \\sim C32-C33 \\sim C35-C34 \\sim C36-C37 \\sim C39-C38 \\sim C40-C41
\\sim C41-C42 \\sim C43-C44
 \\sim C45-C44 \\sim C46-C47 \\sim C47-C48 \\sim C49-C50 \\sim C51-C50 \\sim
C51-C33 \\sim C52-C36 \\sim C53-
 C52 \\sim C54-C53 \\sim C54-C37 \\sim C55-C40 \\sim C56-C55 \\sim C56-C42
\\sim C58-C59 \\sim C58-C57 ~
 C60-C61 \\sim C60-C59 \\sim C61-C57
 with sigma of 0.02
 C33-C49 \\sim C40-C42 \\sim C52-C54 \\sim C57-C60 \\sim C33-C50 \\sim C36-C54
\\sim C37-C52 \\sim C40-C56
 \\sim C42-C55 \\sim C49-C51 \\sim C57-C59 \\sim C58-C60 \\sim C32-C50 \\sim
C32-C51 \\sim C36-C53 \\sim C37-
 C53 \\sim C41-C55 \\sim C41-C56 \\sim C43-C45 \\sim C46-C48 \\sim C58-C61
\\sim C59-C61
 with sigma of 0.04
 C32-C48 \\sim C32-C34 \\sim C33-C35 \\sim C33-C52 \\sim C35-C52 \\sim C38-C54
\\sim C38-C40 \\sim C39-C41
 \\sim C40-C54 \\sim C41-C43 \\sim C42-C57 \\sim C42-C44 \\sim C44-C57 \\sim
C45-C58 \\sim C46-C59 \\sim C47-
 C49 \\sim C47-C60 \\sim C49-C60 \\sim C50-C61 \\sim C51-C53 \\sim C53-C55
\\sim C56-C61 \\sim C35-C37 ~
 C36-C38 \\sim C44-C46 \\sim C44-C59 \\sim C45-C47 \\sim C47-C58 \\sim C50-C52
\\sim C51-C60 \\sim C52-C61
 \\sim C53-C57 \\sim C53-C60 \\sim C54-C56 \\sim C54-C61 \\sim C55-C57 \\sim
C34-C36 \\sim C34-C51 \\sim C36-
 C51 \\sim C37-C39 \\sim C37-C55 \\sim C39-C55 \\sim C43-C56 \\sim C43-C58
\\sim C48-C50 \\sim C48-C59 ~
 C50-C59 \\sim C56-C58
 with sigma of 0.04
3. Restrained planarity
 C32, C49, C50, C51
 with sigma of 0.1
 C33, C34, C51, C52
 with sigma of 0.1
 C33, C49, C50, C51
 with sigma of 0.1
 C35, C36, C51, C52
 with sigma of 0.1
 C37, C52, C53, C54
 with sigma of 0.1
 C40, C41, C55, C56
 with sigma of 0.1
 C40, C41, C42, C55
 with sigma of 0.1
 C42, C43, C56, C57
 with sigma of 0.1
 C42, C43, C44, C58
 with sigma of 0.1
 C47, C48, C49, C59
 with sigma of 0.1
 C47, C48, C49, C50
 with sigma of 0.1
 C50, C53, C60, C61
 with sigma of 0.1
 C51, C52, C53, C61
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
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: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 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
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H00l(0.5) H00m(0.5) H00n(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)
7.a Riding coordinates:
 C00H(H00a,H00b,H00h)
7.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G)
7.c Idealised Me refined as rotating group:
 C00M(H00i,H00j,H00k), C00N(H00l,H00m,H00n)
;
_shelx_res_checksum              44419
_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 1.928
_oxdiff_exptl_absorpt_empirical_full_min 0.577