Bulky metallocavitands with a chiral cavity constructed by aluminum and magnesium atrane-likes: enantioselective recognition and separation of racemic alcohols.
Li, Yingguo; Yu, Dawei; Dai, Zhongran; Zhang, Jinjin; Shao, Yongliang; Tang, Ning; Wu, Jincai; Dalton transactions (Cambridge, England : 2003) 44 (2015) 5692–5702; doi:10.1039/c4dt03848g

data_7033985
_publ_section_title
;
 Bulky metallocavitands with a chiral cavity constructed by aluminum and
 magnesium atrane-likes: enantioselective recognition and separation of
 racemic alcohols.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5692
_journal_page_last               5702
_journal_paper_doi               10.1039/c4dt03848g
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C120 H165 Mg4 N3 O15'
_chemical_formula_sum            'C120 H165 Mg4 N3 O15'
_chemical_formula_weight         1986.79
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-01-21 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   21.817(3)
_cell_length_b                   21.817(3)
_cell_length_c                   16.960(3)
_cell_measurement_reflns_used    2562
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      28.4680
_cell_measurement_theta_min      3.0889
_cell_volume                     6991.1(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_details
;
  1 omega   17.00   78.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305 -128.0000  -65.0000 61

  2 omega  -46.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  -77.0000  -30.0000 97
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0006821000
_diffrn_orient_matrix_UB_12      0.0321395000
_diffrn_orient_matrix_UB_13      0.0026397000
_diffrn_orient_matrix_UB_21      0.0375220000
_diffrn_orient_matrix_UB_22      0.0193615000
_diffrn_orient_matrix_UB_23      0.0004808000
_diffrn_orient_matrix_UB_31      0.0002993000
_diffrn_orient_matrix_UB_32      0.0022013000
_diffrn_orient_matrix_UB_33      -0.0416995000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.1244
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20450
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         3.10
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    0.944
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_platon_squeeze_details
;
one disordered protonated triethyl amine cation
and other disordered things can not modelled.
;
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.8(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         10342
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.0897
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2538
_reflns_number_gt                4669
_reflns_number_total             10342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03848g2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7033982--7033987.cif.'
_cod_database_code               7033985
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C34-H5
 1.992074 with sigma of 0.02
 Mg4-H5
 2.735796 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C32(H32)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5A), C20(H20), C3(H3), C34(H34), C39(H39), C18(H18), C40(H40), C36(H36),
 C37(H37), C38(H38)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C33(H33A,H33B,H33C), C11(H11A,H11B,
 H11C), C14(H14A,H14B,H14C), C25(H25A,H25B,H25C), C15(H15A,H15B,H15C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C24(H24A,H24B,H24C),
 C29(H29A,H29B,H29C), C13(H13A,H13B,H13C)
;
_olex2_submission_special_instructions 'No special instructions were received'