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_7045868
_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 Ni5 O12, 4(Cl1 O4), 3.5 C H4 O'
_chemical_formula_sum            'C79 H100 Cl4 Cr2 N12 Ni5 O35'
_chemical_formula_weight         2317.05
_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     direct
_audit_creation_date             2016-04-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_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                   14.6131(3)
_cell_length_b                   14.6131(3)
_cell_length_c                   37.2857(9)
_cell_measurement_reflns_used    7987
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.181
_cell_measurement_theta_min      2.714
_cell_volume                     6895.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       APE2
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      120.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEXII diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            26509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.339
_diffrn_reflns_theta_min         1.638
_diffrn_source                   Mo
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0665 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.7879.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       block
_exptl_crystal_F_000             3582
_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
_platon_squeeze_details          '3.5 MeOH per asymmetric unit'
_refine_diff_density_max         0.976
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0985P)^2^+35.3976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2044
_reflns_number_total             2823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00685g2.cif
_cod_data_source_block           1
_cod_database_code               7045868
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.654
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Ni1, Cr1}
3. Uiso/Uaniso restraints and constraints
Uanis(Ni1) = Uanis(Cr1)
4. Others
 Fixed Sof: Ni1(0.66666) Cr1(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              6105
_shelx_fab_checksum              10743
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-11
_olex2_date_sample_submission    2016-04-11
_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 527o
_olex2_submission_special_instructions 'No special instructions were received'