Aluminium nanorings: configuration deformation and structural transformation.
Geng, Lin; Li, Qiao-Hong; Wang, San-Tai; Liu, Ya-Jie; Fang, Wei-Hui; Zhang, Jian; Chemical communications (Cambridge, England) 57 (2021) 2085–2088; doi:10.1039/d0cc07513b

data_7127847
_publ_section_title
;
 Aluminium nanorings: configuration deformation and structural
 transformation.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2085
_journal_page_last               2088
_journal_paper_doi               10.1039/d0cc07513b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H130 Al10 O40'
_chemical_formula_sum            'C60 H130 Al10 O40'
_chemical_formula_weight         1761.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-18 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1044(2)
_cell_length_b                   15.8179(2)
_cell_length_c                   28.5609(3)
_cell_measurement_reflns_used    14584
_cell_measurement_temperature    100.6(8)
_cell_measurement_theta_max      53.7470
_cell_measurement_theta_min      2.6620
_cell_volume                     4111.48(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.6(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.978
_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     -9.00  31.28   0.38    0.10    --   -1.25  54.00-125.00  106
  2  \w    -60.00 -22.00   0.38    0.10    --   -1.25 -54.00  91.00  100
  3  \w     10.00  36.22   0.38    0.50    --   59.21 -54.00  91.00   69
  4  \w     63.00  88.08   0.38    0.50    --   59.21  54.00-125.00   66
  5  \w    -62.00   9.06   0.38    0.50    --  -61.71  54.00-125.00  187
  6  \w   -133.00 -45.98   0.38    0.50    --  -61.71 -54.00  91.00  229
  7  \w    -16.00  36.06   0.38    0.10    --   -1.25  57.00   0.00  137
  8  \w     40.00  69.64   0.38    0.10    --   -1.25  57.00   0.00   78
  9  \w    -14.00  43.00   0.38    0.50    --   59.21 -38.00 120.00  150
 10  \w     -3.00  24.36   0.38    0.50    --   59.21 -19.00 150.00   72
 11  \w     79.00 114.72   0.38    0.50    --   59.21 125.00 120.00   94
 12  \w    -62.00 -35.78   0.38    0.50    --  -61.71  57.00  30.00   69
 13  \w   -133.00 -82.84   0.38    0.50    --  -61.71-125.00-120.00  132
 14  \w    -81.00 -20.96   0.38    0.50    --  -61.71 125.00-120.00  158
 15  \w    -25.00   6.16   0.38    0.50    --  -61.71  19.00  90.00   82
 16  \w    -31.00  10.04   0.38    0.50    --  -61.71  57.00  30.00  108
 17  \w    -26.00   9.34   0.38    0.50    --  -61.71  19.00-180.00   93
 18  \w   -134.00 -86.12   0.38    0.50    --  -61.71-125.00-180.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0579672000
_diffrn_orient_matrix_UB_12      -0.0529111000
_diffrn_orient_matrix_UB_13      -0.0321087000
_diffrn_orient_matrix_UB_21      0.1120314000
_diffrn_orient_matrix_UB_22      0.0160430000
_diffrn_orient_matrix_UB_23      -0.0280881000
_diffrn_orient_matrix_UB_31      0.0758763000
_diffrn_orient_matrix_UB_32      -0.0641052000
_diffrn_orient_matrix_UB_33      0.0194779000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            28684
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         53.895
_diffrn_reflns_theta_min         3.626
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0652
_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^)+(0.1215P)^2^+1.8409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5546
_reflns_number_total             7301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07513b2.cif
_cod_data_source_block           AlOC-35
_cod_depositor_comments
'Adding full bibliography for 7127841--7127847.cif.'
_cod_database_code               7127847
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al O C'
_reflns_odcompleteness_completeness 88.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C41_$1-C42
 2.2 with sigma of 0.01
 C42A-C32A
 3.1 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C41: within 4.5A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C16) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C15A)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C20A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C30A)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C42A) \\sim Ueq,
Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C15(0.65) H15A(0.65) H15B(0.65) C16(0.48) H16A(0.48) H16B(0.48)
 C16A(0.52) H16C(0.52) H16D(0.52) C20A(0.65) H20A(0.65) H20B(0.65) C19(0.65)
 H19A(0.65) H19B(0.65) H19C(0.65) C20(0.35) H20C(0.35) H20D(0.35) C24A(0.6)
 H24A(0.6) H24B(0.6) C23A(0.7) H23A(0.7) H23B(0.7) H23C(0.7) C23(0.3) H23D(0.3)
 H23E(0.3) H23F(0.3) C24(0.4) H24C(0.4) H24D(0.4) C26A(0.58) H26A(0.58)
 H26B(0.58) H26C(0.58) C26(0.42) H26D(0.42) H26E(0.42) H26F(0.42) C15A(0.35)
 H15C(0.35) H15D(0.35) H28A(0.65) H28B(0.65) H28C(0.65) H28D(0.35) H28E(0.35)
 H28F(0.35) C19A(0.35) H19D(0.35) H19E(0.35) H19F(0.35) C30(0.64) H30A(0.64)
 H30B(0.64) C30A(0.36) H30C(0.36) H30D(0.36) C32(0.59) H32A(0.59) H32B(0.59)
 C33(0.65) H33A(0.65) H33B(0.65) C34(0.35) H34A(0.35) H34B(0.35) C32A(0.41)
 H32D(0.41) H32C(0.41) C36(0.73) H36A(0.73) H36B(0.73) C36A(0.27) H36C(0.27)
 H36D(0.27) C39A(0.33) H39A(0.33) H39B(0.33) H39C(0.33) C39(0.67) H39D(0.67)
 H39E(0.67) H39F(0.67) H40D(0.73) H40E(0.73) H40F(0.73) H40A(0.27) H40B(0.27)
 H40C(0.27) H41A(0.72) H41B(0.72) H41C(0.72) H41D(0.28) H41E(0.28) H41F(0.28)
 C42(0.52) H42A(0.52) H42B(0.52) H42C(0.52) C42A(0.48) H42D(0.48) H42E(0.48)
 H42F(0.48)
5.a Riding coordinates:
 C28(H28A,H28B,H28C), C28(H28D,H28E,H28F), C33(H33A,H33B), C39A(H39A,H39B,
 H39C), C40(H40D,H40E,H40F), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C41(H41D,
 H41E,H41F), C42(H42A,H42B,H42C), C42A(H42D,H42E,H42F)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7B,H7A), C9(H9A,H9B), C15(H15A,H15B), C16(H16A,H16B), C16A(H16C,H16D),
 C20A(H20A,H20B), C20(H20C,H20D), C24A(H24A,H24B), C24(H24C,H24D), C15A(H15C,
 H15D), C30(H30A,H30B), C30A(H30C,H30D), C32(H32A,H32B), C34(H34A,H34B),
 C32A(H32D,H32C), C36(H36A,H36B), C36A(H36C,H36D)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C19(H19A,H19B,
 H19C), C23A(H23A,H23B,H23C), C23(H23D,H23E,H23F), C26A(H26A,H26B,H26C),
 C26(H26D,H26E,H26F), C19A(H19D,H19E,H19F), C39(H39D,H39E,H39F)
;
_shelx_res_checksum              8913
_shelx_fab_checksum              50408
_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 3.385
_oxdiff_exptl_absorpt_empirical_full_min 0.403