Synthesis and Recognition Properties of Enantiomerically Pure Acyclic Cucurbit[n]uril-Type Molecular Containers.
Lu, Xiaoyong; Isaacs, Lyle; Organic letters 17 (2015) 4038–4041; doi:10.1021/acs.orglett.5b01948

data_1529381
_publ_section_title
;
 Synthesis and Recognition Properties of Enantiomerically Pure Acyclic
 Cucurbit[n]uril-Type Molecular Containers.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4038
_journal_page_last               4041
_journal_paper_doi               10.1021/acs.orglett.5b01948
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C108 H134 K N32 O32, 2(C3 H6 O), 13(H2 O)'
_chemical_formula_sum            'C114 H172 Cl K Li0 N47 O38'
_chemical_formula_weight         2883.53
_chemical_name_systematic        'Potassium CB4(acetone) chloride hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 101.1720(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.3719(16)
_cell_length_b                   14.1615(8)
_cell_length_c                   33.7030(18)
_cell_measurement_reflns_used    15284
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.3
_cell_volume                     13753.1(13)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0032031
_diffrn_orient_matrix_UB_12      -0.0691811
_diffrn_orient_matrix_UB_13      0.0058026
_diffrn_orient_matrix_UB_21      0.0223450
_diffrn_orient_matrix_UB_22      -0.0054596
_diffrn_orient_matrix_UB_23      -0.0188120
_diffrn_orient_matrix_UB_31      0.0263575
_diffrn_orient_matrix_UB_32      0.0130434
_diffrn_orient_matrix_UB_33      0.0229582
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            58638
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.765
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6100
_exptl_crystal_id                LXY-2-73
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         12118
_refine_ls_number_restraints     1120
_refine_ls_restrained_S_all      1.328
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0984
_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^)+(0.0200P)^2^+73.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9122
_reflns_number_total             12118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b01948_si_002.cif
_cod_data_source_block           2702
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1529381.cif.
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1529381
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              23242
_shelx_hkl_checksum              40748
_shelx_fab_checksum              67234