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_7127844
_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         'C50 H110 Al10 O40'
_chemical_formula_sum            'C50 H110 Al10 O40'
_chemical_formula_weight         1621.17
_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_date             2021-01-16
_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                 115.686(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.1093(5)
_cell_length_b                   27.0496(6)
_cell_length_c                   7.7076(2)
_cell_measurement_reflns_used    16101
_cell_measurement_temperature    107.3(3)
_cell_measurement_theta_max      59.1620
_cell_measurement_theta_min      2.5230
_cell_volume                     3778.24(19)
_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 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      107.3(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_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     62.00  97.00   0.50    0.45    --   72.34-108.00  89.00   70
  2  \w     98.00 139.00   0.50    0.45    --   72.34 108.00-173.00   82
  3  \w    -98.00 -45.00   0.50    0.45    --  -75.46 108.00-173.00  106
  4  \w   -118.00 -93.00   0.50    0.45    --  -75.46-108.00  89.00   50
  5  \w    -28.00  15.00   0.50    0.11    --   -1.56 -57.00   0.00   86
  6  \w    -55.00  14.00   0.50    0.11    --   -1.56 -57.00-180.00  138
  7  \w    -49.00   6.00   0.50    0.11    --   -1.56 -38.00 120.00  110
  8  \w    -14.00  72.00   0.50    0.11    --   -1.56  38.00 -30.00  172
  9  \w     23.00  56.00   0.50    0.11    --   -1.56  57.00 120.00   66
 10  \w    -18.00  20.00   0.50    0.11    --   -1.56  57.00 120.00   76
 11  \w    -14.00  41.00   0.50    0.11    --   -1.56  38.00-120.00  110
 12  \w    -59.00 -32.00   0.50    0.11    --   -1.56 -57.00   0.00   54
 13  \w    -52.00  12.00   0.50    0.11    --   -1.56 -38.00   0.00  128
 14  \w     49.00  78.00   0.50    0.45    --   72.34  77.00  90.00   58
 15  \w     49.00  77.00   0.50    0.45    --   72.34  77.00  30.00   56
 16  \w     49.00  75.00   0.50    0.45    --   72.34  77.00-120.00   52
 17  \w     58.00 114.00   0.50    0.45    --   72.34  38.00 -90.00  112
 18  \w      0.00  95.00   0.50    0.45    --   72.34 -77.00 -60.00  190
 19  \w      1.00  94.00   0.50    0.45    --   72.34 -77.00  90.00  186
 20  \w     49.00 108.00   0.50    0.45    --   72.34  77.00 -30.00  118
 21  \w     56.00 138.00   0.50    0.45    --   72.34  57.00 150.00  164
 22  \w      1.00  95.00   0.50    0.45    --   72.34 -77.00   0.00  188
 23  \w    114.00 140.00   0.50    0.45    --   72.34  74.00 -44.20   52
 24  \w     49.00  84.00   0.50    0.45    --   72.34  77.00   0.00   70
 25  \w     52.00  79.00   0.50    0.45    --   72.34  68.00 -61.73   54
 26  \w     51.00  77.00   0.50    0.45    --   72.34  71.00  59.12   52
 27  \w     21.00 102.00   0.50    0.45    --   72.34-125.00 120.00  162
 28  \w      1.00  65.00   0.50    0.45    --   72.34 -57.00 -60.00  128
 29  \w    113.00 139.00   0.50    0.45    --   72.34  77.00 -30.00   52
 30  \w    102.00 144.00   0.50    0.45    --   72.34  57.00 -73.52   84
 31  \w     50.00 112.00   0.50    0.45    --   72.34  74.00 -44.20  124
 32  \w     21.00 108.00   0.50    0.45    --   72.34-125.00 -60.00  174
 33  \w     49.00  75.00   0.50    0.45    --   72.34  77.00 -90.00   52
 34  \w     49.00  75.00   0.50    0.45    --   72.34  77.00 -60.00   52
 35  \w     98.00 135.00   0.50    0.45    --   72.34  77.00  90.00   74
 36  \w    102.00 129.00   0.50    0.45    --   72.34  77.00  60.00   54
 37  \w     91.00 145.00   0.50    0.45    --   72.34  77.00 -90.00  108
 38  \w     56.00  87.00   0.50    0.45    --   72.34  57.00 -73.52   62
 39  \w     96.00 144.00   0.50    0.45    --   72.34  77.00-120.00   96
 40  \w     49.00  77.00   0.50    0.45    --   72.34  77.00-180.00   56
 41  \w     96.00 143.00   0.50    0.45    --   72.34  77.00-180.00   94
 42  \w     49.00  79.00   0.50    0.45    --   72.34  77.00  60.00   60
 43  \w    -98.00 -58.00   0.50    0.45    --  -75.46 -62.00 144.53   80
 44  \w    -64.00  -2.00   0.50    0.45    --  -75.46  57.00-180.00  124
 45  \w    -78.00 -52.00   0.50    0.45    --  -75.46 -77.00 -63.87   52
 46  \w    -81.00 -54.00   0.50    0.45    --  -75.46 -70.00-145.55   54
 47  \w   -146.00 -60.00   0.50    0.45    --  -75.46 -46.00-170.84  172
 48  \w    -95.00 -52.00   0.50    0.45    --  -75.46 -77.00  23.43   86
 49  \w    -80.00 -53.00   0.50    0.45    --  -75.46 -77.00-150.00   54
 50  \w   -146.00 -60.00   0.50    0.45    --  -75.46 -60.00  51.82  172
 51  \w   -128.00 -50.00   0.50    0.45    --  -75.46 -80.00 125.41  156
 52  \w   -106.00 -26.00   0.50    0.45    --  -75.46 125.00-180.00  160
 53  \w    -29.00  -2.00   0.50    0.45    --  -75.46  38.00-180.00   54
 54  \w    -86.00 -52.00   0.50    0.45    --  -75.46 -77.00 -90.00   68
 55  \w   -145.00 -59.00   0.50    0.45    --  -75.46 -57.00  30.00  172
 56  \w    -76.00 -50.00   0.50    0.45    --  -75.46 -81.00-159.64   52
 57  \w    -77.00 -52.00   0.50    0.45    --  -75.46 -77.00 150.00   50
 58  \w    -95.00 -56.00   0.50    0.45    --  -75.46 -65.00-161.06   78
 59  \w    -76.00 -51.00   0.50    0.45    --  -75.46 -79.00-100.33   50
 60  \w   -136.00-110.00   0.50    0.45    --  -75.46 -79.00-100.33   52
 61  \w    -81.00 -52.00   0.50    0.45    --  -75.46 -77.00  90.00   58
 62  \w    -78.00 -53.00   0.50    0.45    --  -75.46 -73.00 176.50   50
 63  \w   -134.00-107.00   0.50    0.45    --  -75.46 -73.00 176.50   54
 64  \w    -82.00 -55.00   0.50    0.45    --  -75.46 -68.00 125.73   54
 65  \w    -77.00 -52.00   0.50    0.45    --  -75.46 -77.00-122.20   50
 66  \w   -148.00-122.00   0.50    0.45    --  -75.46 -77.00-122.20   52
;
_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      0.0505860000
_diffrn_orient_matrix_UB_12      0.0357569000
_diffrn_orient_matrix_UB_13      0.0400604000
_diffrn_orient_matrix_UB_21      0.0460510000
_diffrn_orient_matrix_UB_22      -0.0321833000
_diffrn_orient_matrix_UB_23      -0.0233213000
_diffrn_orient_matrix_UB_31      -0.0279349000
_diffrn_orient_matrix_UB_32      0.0116885000
_diffrn_orient_matrix_UB_33      -0.1872119000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            53526
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.904
_diffrn_reflns_theta_min         2.552
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74880
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3931
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0718P)^2^+5.0632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3346
_reflns_number_total             3931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07513b2.cif
_cod_data_source_block           AlOC-34
_cod_depositor_comments
'Adding full bibliography for 7127841--7127847.cif.'
_cod_original_cell_volume        3778.24(18)
_cod_database_code               7127844
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Al C O'
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.879
_reflns_odcompleteness_completeness 100.00
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C10A
 1.3 with sigma of 0.01
 H9A-C17
 1.7 with sigma of 0.01
 H9B-C17
 1.61 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C10A) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5) H8AA(0.8) H8AB(0.8) H8BC(0.2) H8BD(0.2)
 C10(0.8) H10A(0.8) H10B(0.8) H10C(0.8) C13A(0.18) H13A(0.18) H13B(0.18)
 H13C(0.18) C12(0.8) H12A(0.8) H12B(0.8) H12C(0.8) C13(0.82) H13D(0.82)
 H13E(0.82) H13F(0.82) C14(0.58) H14A(0.58) H14B(0.58) H14C(0.58) C14A(0.42)
 H14D(0.42) H14E(0.42) H14F(0.42) C12A(0.2) H12D(0.2) H12E(0.2) H12F(0.2)
 C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C10A(0.2) H10D(0.2) H10E(0.2) H10F(0.2)
 C19(0.325) H19A(0.325) H19B(0.325) H19C(0.325) C19A(0.175) H19D(0.175)
 H19E(0.175) H19F(0.175) H9A(0.5) H9B(0.5)
5.a Riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8AA,H8AB), C8(H8BC,H8BD)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C13A(H13A,H13B,H13C), C12(H12A,H12B,
 H12C), C13(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F),
 C12A(H12D,H12E,H12F), C17(H17A,H17B,H17C), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              80065
_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 1.880
_oxdiff_exptl_absorpt_empirical_full_min 0.664