Order in disorder: solution and solid-state studies of [MIII2MII5] wheels (MIII = Cr, Al; MII = Ni, Zn)
Fraser, Hector; Nichol, Gary Stephen; Uhrin, Dusan; Nielsen, Ulla Gro; Evangelisti, Marco; Schnack, Jürgen; Brechin, Euan K.; Dalton Transactions  (2018) –; doi:10.1039/C8DT00685G

data_7045869
_publ_section_title
;
 Order in disorder: solution and solid-state studies of [MIII2MII5] wheels
 (MIII = Cr, Al; MII = Ni, Zn)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT00685G
_journal_year                    2018
_chemical_formula_moiety
'C72 H72 Al2 N12 O12 Zn5, 4(Cl1 O4), 8 C H4 O'
_chemical_formula_sum            'C80 H104 Al2 Cl4 N12 O36 Zn5'
_chemical_formula_weight         2332.36
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-01-24 deposited with the CCDC.
2018-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.4962(5)
_cell_length_b                   14.4962(5)
_cell_length_c                   38.022(2)
_cell_measurement_reflns_used    3072
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      26.3140
_cell_measurement_theta_min      3.2870
_cell_volume                     6919.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -14.00  13.00   1.00   30.00    --   -9.43  38.00 -90.00   27
  2  \w    -62.00  38.00   1.00   30.00    --   10.92 -77.00-120.00  100
  3  \w      7.00  39.00   1.00   30.00    --   10.92  57.00 150.00   32
  4  \w    -37.00   5.00   1.00   30.00    --   10.92 -38.00 -30.00   42
  5  \w    -27.00   1.00   1.00   30.00    --   10.92 -38.00  30.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0077818000
_diffrn_orient_matrix_UB_12      -0.0025007000
_diffrn_orient_matrix_UB_13      -0.0183138000
_diffrn_orient_matrix_UB_21      -0.0559547000
_diffrn_orient_matrix_UB_22      -0.0288740000
_diffrn_orient_matrix_UB_23      -0.0025618000
_diffrn_orient_matrix_UB_31      -0.0000322000
_diffrn_orient_matrix_UB_32      0.0484959000
_diffrn_orient_matrix_UB_33      -0.0024501000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            13554
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.810
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_correction_T_min  0.7260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0706 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.7319. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       plate
_exptl_crystal_F_000             3600
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0403P)^2^+65.7332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2492
_reflns_number_total             3142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00685g2.cif
_cod_data_source_block           4
_cod_original_cell_volume        6919.4(6)
_cod_database_code               7045869
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C30 H30 N10 O10 Zn Cl Al'
_chemical_oxdiff_usercomment     '@ 120 K 805o'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.744(2) 0.256(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Shared sites
{Zn1, Al1}
4. Uiso/Uaniso restraints and constraints
Uanis(Zn1) = Uanis(Al1)
5. Others
 Fixed Sof: Zn1(0.66666) Al1(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_shelx_res_checksum              71784
_shelx_fab_checksum              31780
_olex2_date_sample_data_collection 2017-01-13
_olex2_date_sample_submission    2017-01-11
_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 805o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.884