Kinetic Study of Chiral Intermolecular Interactions by Moment Analysis Based on Affinity Capillary Electrophoresis.
Suzuki, Nozomu; Kinoshita, Mariko; Miyabe, Kanji; Analytical chemistry 90 (2018) 11048–11053; doi:10.1021/acs.analchem.8b02823

data_1552962
_publ_section_title
;
 Kinetic Study of Chiral Intermolecular Interactions by Moment Analysis
 Based on Affinity Capillary Electrophoresis.
;
_journal_issue                   18
_journal_name_full               'Analytical chemistry'
_journal_page_first              11048
_journal_page_last               11053
_journal_paper_doi               10.1021/acs.analchem.8b02823
_journal_volume                  90
_journal_year                    2018
_chemical_formula_sum            'C51 H80 O38'
_chemical_formula_weight         1301.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 110.6520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6610(5)
_cell_length_b                   24.3629(7)
_cell_length_c                   15.4291(4)
_cell_measurement_reflns_used    262
_cell_measurement_temperature    93.(2)
_cell_measurement_theta_max      35.6266
_cell_measurement_theta_min      3.1018
_cell_volume                     6563.9(3)
_computing_cell_refinement       'APEX3 v2015.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26127
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.528
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         10753
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0625
_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^)+(0.1118P)^2^+15.3453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1728
_reflns_number_gt                10690
_reflns_number_total             10753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac8b02823_si_001.cif
_cod_data_source_block           RSPPA_bCD
_cod_database_code               1552962
_shelx_res_checksum              5472
_shelx_hkl_checksum              44336
_shelx_fab_checksum              81064