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_7045871
_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 Cr2 N12 O12 Zn5, 5.91(Cl0.68 O2.71), 9 C H4 O'
_chemical_formula_sum            'C81 H108 Cl4 Cr2 N12 O37 Zn5'
_chemical_formula_weight         2414.44
_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             2016-09-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_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                   14.5920(3)
_cell_length_b                   14.5920(3)
_cell_length_c                   37.7623(14)
_cell_measurement_reflns_used    12927
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.4140
_cell_measurement_theta_min      3.3900
_cell_volume                     6963.4(3)
_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 0.999
_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    -20.00  33.00   1.00   20.00    --   -7.39 -99.00-120.00   53
  2  \w    -20.00  33.00   1.00   20.00    --   -7.39 -99.00 -30.00   53
  3  \w    -80.00  15.00   1.00   20.00    --   -7.39 -38.00-120.00   95
  4  \w    -20.00  49.00   1.00   20.00    --    8.80 -99.00  30.00   69
  5  \w    -64.00  -1.00   1.00   20.00    --    8.80 -38.00   0.00   63
  6  \w     -1.00  48.00   1.00   20.00    --    8.80 -99.00  90.00   49
  7  \w    -14.00  77.00   1.00   20.00    --    8.80  38.00 -60.00   91
  8  \w    -36.00  -9.00   1.00   20.00    --    8.80 -77.00  90.00   27
  9  \w     -6.00  79.00   1.00   20.00    --    8.80  19.00-150.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0064305000
_diffrn_orient_matrix_UB_12      -0.0194777000
_diffrn_orient_matrix_UB_13      0.0175729000
_diffrn_orient_matrix_UB_21      -0.0519410000
_diffrn_orient_matrix_UB_22      -0.0075657000
_diffrn_orient_matrix_UB_23      0.0004157000
_diffrn_orient_matrix_UB_31      -0.0202680000
_diffrn_orient_matrix_UB_32      -0.0520727000
_diffrn_orient_matrix_UB_33      -0.0066330000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            35087
_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         25.350
_diffrn_reflns_theta_min         2.792
_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    1.706
_exptl_absorpt_correction_T_max  0.9900
_exptl_absorpt_correction_T_min  0.8357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0701 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.8441.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       plate
_exptl_crystal_F_000             3720
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.903
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2846
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0247P)^2^+127.7921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2599
_reflns_number_total             2846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00685g2.cif
_cod_data_source_block           2
_cod_original_cell_volume        6963.4(4)
_cod_database_code               7045871
_chemical_oxdiff_formula         'C30 H30 N10 O10 Zn Cl Cr'
_chemical_oxdiff_usercomment     '@ 120 K 713o'
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.610
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Cr1, Zn1}
3. Restrained distances
 Cl1-O4 \\sim Cl1-O3 \\sim Cl1A-O3A \\sim Cl1A-O4A \\sim Cl2-O5 \\sim Cl2-O6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Cr1) = Uanis(Zn1)
5. Rigid body (RIGU) restrains
 Cl1A, O3A, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O3A)=1-FVAR(1)
 Sof(Cl1A)=Sof(O4A)=0.33333*(1-FVAR(2))
 Sof(Cl1)=Sof(O4)=0.33333*FVAR(2)
 Sof(O3)=FVAR(1)
 Fixed Sof: Zn1(0.66666) Cr1(0.3333)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
7.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              66304
_shelx_fab_checksum              7612
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-09-20
_olex2_date_sample_submission    2016-09-20
_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 713o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.886