A [Mn<sub>18</sub>] wheel-of-wheels.
Coletta, Marco; Tziotzi, Thomais G.; Gray, Mark; Nichol, Gary S.; Singh, Mukesh K.; Milios, Constantinos J.; Brechin, Euan K.; Chemical communications (Cambridge, England) 57 (2021) 4122–4125; doi:10.1039/d1cc00185j

data_7128057
_publ_section_title
;
 A [Mn<sub>18</sub>] wheel-of-wheels.
;
_journal_issue                   34
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4122
_journal_page_last               4125
_journal_paper_doi               10.1039/d1cc00185j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H130 Br12 Mn18 N18 O32, 10[CH4O]'
_chemical_formula_sum            'C70 H170 Br12 Mn18 N18 O42'
_chemical_formula_weight         3884.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-08
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-08 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.126(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.408(6)
_cell_length_b                   23.209(7)
_cell_length_c                   30.524(12)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      20.252
_cell_measurement_theta_min      2.395
_cell_volume                     13041(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Diamond Light Source I-19 EH1'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_unetI/netI     0.1490
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46537
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        20.147
_diffrn_reflns_theta_max         20.147
_diffrn_reflns_theta_min         1.068
_diffrn_source                   Synchrotron
_diffrn_source_current           0.0
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_power             0.0
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.989
_exptl_absorpt_correction_T_max  0.4282
_exptl_absorpt_correction_T_min  0.2247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1459 before and 0.0974 after correction.
The Ratio of minimum to maximum transmission is 0.5248.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       plate
_exptl_crystal_F_000             7688
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         6837
_refine_ls_number_restraints     961
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.1166
_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^)+(0.1305P)^2^+309.7215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3142
_refine_ls_wR_factor_ref         0.3477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4506
_reflns_number_total             6837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00185j2.cif
_cod_data_source_block           mc660
_cod_depositor_comments          'Adding full bibliography for 7128057.cif.'
_cod_original_cell_volume        13041(7)
_cod_database_code               7128057
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.781
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H10 of O10
 At 1.5 times of:
  All C(H,H,H) groups, H5 of O5
2. Restrained distances
 C18-C17 = C9-C10 = C6-C5 = C15-C16
 1.45 with sigma of 0.01
 O10-H10
 0.84 with sigma of 0.02
 Mn7-H10
 2.4 with sigma of 0.04
 H10-Mn1
 2.4 with sigma of 0.04
3. Rigid body (RIGU) restrains
 Br1, Br2, Br3, Br4, Br5, Br6, Mn1, Mn2, Mn3, Mn4, Mn5, Mn6, Mn7, Mn8, Mn9, O1,
  O2, O3, O4, O5, O6, O7, O8, O9, O10, O11, O12, O13, O14, O15, O16, N1, N2, N3,
  N4, N5, N6, N7, N8, N9, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12,
 C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28,
  C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B)
4.b Tetrahedral OH refined with riding coordinates:
 O5(H5)
4.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23896
_shelx_hkl_checksum              45356
_shelx_fab_checksum              75868
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id MC660
_olex2_submission_special_instructions 'No special instructions were received'