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_7045870
_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 Ni5 O12, 4(Cl1 O4), 9 C H4 O'
_chemical_formula_sum            'C81 H108 Al2 Cl4 N12 Ni5 O37'
_chemical_formula_weight         2331.10
_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             2016-11-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_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                   14.53160(10)
_cell_length_b                   14.53160(10)
_cell_length_c                   37.9260(9)
_cell_measurement_reflns_used    20349
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.3420
_cell_measurement_theta_min      4.1950
_cell_volume                     6935.77(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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 0.987
_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    -66.00  29.00   1.00   10.00    --  -43.17  38.00 -90.00   95
  2  \w    -70.00  27.00   1.00   10.00    --  -43.17  57.00  90.00   97
  3  \w   -100.00  -7.00   1.00   10.00    --  -43.17 133.00 -49.00   93
  4  \w    -66.00  29.00   1.00   10.00    --  -43.17  38.00-180.00   95
  5  \w   -113.00 -17.00   1.00   10.00    --  -43.17 -57.00 -60.00   96
  6  \w     23.00  98.00   1.00   10.00    --   43.17-125.00-120.00   75
  7  \w     41.00 128.00   1.00   30.00    --  111.00-137.00  64.00   87
  8  \w     83.00 178.00   1.00   30.00    --  111.00  61.00 -30.00   95
  9  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00  60.00   79
 10  \w     94.00 178.00   1.00   30.00    --  111.00 125.00-180.00   84
 11  \w     37.00 142.00   1.00   30.00    --  111.00 -77.00 -60.00  105
 12  \w     39.00 121.00   1.00   30.00    --  111.00-125.00 -30.00   82
 13  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00  90.00   79
 14  \w     83.00 178.00   1.00   30.00    --  111.00  61.00-180.00   95
 15  \w     30.00 109.00   1.00   30.00    --  111.00 -94.00 150.00   79
 16  \w     41.00 139.00   1.00   30.00    --  111.00 -61.00-180.00   98
 17  \w     39.00 121.00   1.00   30.00    --  111.00-125.00  30.00   82
 18  \w     39.00 121.00   1.00   30.00    --  111.00-125.00 -90.00   82
 19  \w     39.00 121.00   1.00   30.00    --  111.00-125.00 150.00   82
 20  \w     87.00 161.00   1.00   30.00    --  111.00  45.00 -60.00   74
 21  \w     72.00 125.00   1.00   30.00    --  111.00-133.00-117.00   53
 22  \w    109.00 153.00   1.00   30.00    --  111.00  61.00-120.00   44
 23  \w     81.00 106.00   1.00   30.00    --  111.00  77.00-120.00   25
 24  \w    118.00 176.00   1.00   30.00    --  111.00  77.00-120.00   58
 25  \w     67.00 108.00   1.00   30.00    --  111.00 -94.00  30.00   41
 26  \w     55.00  85.00   1.00   30.00    --  111.00 -94.00 120.00   30
 27  \w    133.00 159.00   1.00   30.00    --  111.00 125.00 -90.00   26
 28  \w     55.00  81.00   1.00   30.00    --  111.00-125.00  60.00   26
 29  \w    112.00 156.00   1.00   30.00    --  111.00 -15.00  60.00   44
 30  \w     34.00  96.00   1.00   30.00    --  111.00 -15.00  60.00   62
;
_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      -0.0125820000
_diffrn_orient_matrix_UB_12      -0.0182141000
_diffrn_orient_matrix_UB_13      0.0401524000
_diffrn_orient_matrix_UB_21      0.0000989000
_diffrn_orient_matrix_UB_22      0.1053696000
_diffrn_orient_matrix_UB_23      0.0046000000
_diffrn_orient_matrix_UB_31      -0.1217544000
_diffrn_orient_matrix_UB_32      -0.0595794000
_diffrn_orient_matrix_UB_33      -0.0041674000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            32013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.591
_diffrn_reflns_theta_min         3.700
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.195
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0943 before and 0.0760 after correction.
The Ratio of minimum to maximum transmission is 0.6782.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       plate
_exptl_crystal_F_000             3624
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.089
_platon_squeeze_details
'approx 27 molecules of MeOH per unit cell masked with SQUEEZE'
_refine_diff_density_max         0.878
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0818
_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^)+(0.1395P)^2^+42.4831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2373
_refine_ls_wR_factor_ref         0.2395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3044
_reflns_number_total             3217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00685g2.cif
_cod_data_source_block           3
_cod_original_cell_volume        6935.77(19)
_cod_database_code               7045870
_chemical_oxdiff_formula         'C30 H30 N10 O10 Ni Cl Al'
_chemical_oxdiff_usercomment     '@ 120 K 754o SOC'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Ni1, Al1}
3. Uiso/Uaniso restraints and constraints
Uanis(Ni1) = Uanis(Al1)
4. Others
 Fixed Sof: Ni1(0.66667) Al1(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
5.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              88819
_shelx_fab_checksum              12637
_shelx_shelxl_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-11
_olex2_date_sample_submission    2016-10-14
_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 '754o SOB'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 2.062
_oxdiff_exptl_absorpt_empirical_full_min 0.626
_platon_squeeze_void_probe_radius 1.20