Enantiospecific recognition of 2-butanol by an inherently chiral cavitand in the solid state
Pinalli, Roberta; Brancatelli, Giovanna; Nicosia, Carlo; Barboza, Tahnie; Guy, Laure; Dutasta, Jean-Pierre; De Zorzi, Rita; Demitri, Nicola; Dalcanale, Enrico; Geremia, Silvano; CrystEngComm  (2017) –; doi:10.1039/C7CE00557A

data_7228321
_publ_section_title
;
 Enantiospecific recognition of 2-butanol by an inherently chiral cavitand
 in the solid state
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00557A
_journal_year                    2017
_chemical_formula_moiety         'C55 H49 O10 P3 S, 2.7(C4 H10 O), H2 O'
_chemical_formula_sum            'C65.8 H78 O13.7 P3 S'
_chemical_formula_weight         1213.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-05-10 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.99(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.150(5)
_cell_length_b                   15.847(3)
_cell_length_c                   31.397(6)
_cell_measurement_reflns_used    237
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.494
_cell_measurement_theta_min      2.184
_cell_volume                     11926(4)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Ortep3 for Windows'
_computing_publication_material  enCIFer/publCIF
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'Sir2014 (Burla, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9333
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        44.494
_diffrn_reflns_theta_max         44.494
_diffrn_reflns_theta_min         2.184
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       'Small blocks'
_exptl_crystal_F_000             5147
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         9333
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.1031
_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^)+(0.1256P)^2^+92.9606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2556
_refine_ls_wR_factor_ref         0.2622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8558
_reflns_number_total             9333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00557a2.cif
_cod_data_source_block           2PO1PSMe2ButOH
_cod_original_cell_volume        11927(4)
_cod_database_code               7228321
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.848
_shelx_res_checksum              97776
_shelx_fab_checksum              34408