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_7127843
_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         'C56 H92 Al10 F2 O48'
_chemical_formula_sum            'C56 H92 Al10 F0.5 O50'
_chemical_formula_weight         1844.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-01-07
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2020.12.01 svn.rb'be22f01f' for OlexSys, GUI svn.r6224)
;
_audit_update_record
;
2021-01-20 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.372(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.8191(6)
_cell_length_b                   16.1753(4)
_cell_length_c                   15.5044(5)
_cell_measurement_reflns_used    8754
_cell_measurement_temperature    101.2(7)
_cell_measurement_theta_max      60.0670
_cell_measurement_theta_min      2.6750
_cell_volume                     4628.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      101.2(7)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  62.50   0.70    0.30    --   -1.25  49.00 -12.00   95
  2  \w     21.00  46.90   0.70    0.30    --   -1.25  57.00  90.00   37
  3  \w      1.00  35.30   0.70    4.00    --   72.65 -57.00  30.00   49
  4  \w     37.00  65.00   0.70    4.00    --   72.65 -57.00  30.00   40
  5  \w      0.00  26.60   0.70    4.00    --   72.65 -19.00 -90.00   38
  6  \w      3.00  28.20   0.70    4.00    --   72.65 -49.00-159.00   36
  7  \w    -21.00  11.90   0.70    0.30    --   -1.25 -49.00-159.00   47
  8  \w    -69.00 -25.60   0.70    0.30    --   -1.25 -49.00-159.00   62
  9  \w    -51.00  -2.00   0.70    4.00    --  -75.15  49.00 -12.00   70
 10  \w    -43.00 -16.40   0.70    4.00    --  -75.15  38.00  60.00   38
 11  \w    -27.00  -1.80   0.70    4.00    --  -75.15  19.00  90.00   36
 12  \w    -27.00  -0.40   0.70    4.00    --  -75.15  19.00 150.00   38
 13  \w    -27.00  -0.40   0.70    4.00    --  -75.15  19.00 120.00   38
 14  \w    -36.00  -5.90   0.70    4.00    --  -75.15  38.00 150.00   43
 15  \w    -65.00 -11.80   0.70    4.00    --  -75.15  57.00 -60.00   76
 16  \w    -39.00  -5.40   0.70    4.00    --  -75.15  38.00 -60.00   48
 17  \w    -42.30  -1.00   0.70    4.00    --  -75.15  38.00-180.00   59
 18  \w    -27.00  -1.80   0.70    4.00    --  -75.15  19.00-180.00   36
 19  \w   -148.00 -62.60   0.70    4.00    --  -75.15 -49.00-159.00  122
 20  \w     81.00 115.30   0.70    4.00    --   72.65 125.00-150.00   49
 21  \w    120.00 144.50   0.70    4.00    --   72.65 125.00-150.00   35
 22  \w     75.00 113.50   0.70    4.00    --   72.65  49.00 -12.00   55
 23  \w      5.00  62.40   0.70    4.00    --   72.65 -57.00  60.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6857
_diffrn_reflns_point_group_measured_fraction_full 0.807
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         53.846
_diffrn_reflns_theta_min         2.661
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       'clear light colourless'
_exptl_crystal_F_000             1925
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 2049 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.22(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6857
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+6.7531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.553
_reflns_Friedel_fraction_full    0.599
_reflns_Friedel_fraction_max     0.597
_reflns_number_gt                6405
_reflns_number_total             6857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07513b2.cif
_cod_data_source_block           AlOC-38
_cod_depositor_comments
'Adding full bibliography for 7127841--7127847.cif.'
_cod_original_formula_sum        'C56 H92 Al10 F0.50 O50'
_cod_database_code               7127843
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.891
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.773(4)
 0.227(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
O41 \\sim F27: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3A
O45: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
3.8A
O37: within 6.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
6.5A
C37: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 5A
C41: within 5.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
5.5A
Uanis(F27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O37) = Uanis(F26)
4. Rigid body (RIGU) restrains
 Al10, F27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Riding coordinates:
 C47(H47A,H47B,H47C)
5.b Ternary CH refined with riding coordinates:
 C33(H33), C36(H36)
5.c Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B)
5.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              63029
_shelx_fab_checksum              21454
_platon_squeeze_void_probe_radius 1.20
_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
;