Synthesis of per(5-N-carboxamide-5-dehydroxylmethyl)-β-cyclodextrins and their selective recognition ability utilizing multiple hydrogen bonds
Nakamura, Takashi; Yonemura, Sota; Nabeshima, Tatsuya; Chemical Communications  (2019) –; doi:10.1039/C9CC00517J

data_7123013
_publ_section_title
;
 Synthesis of per(5-N-carboxamide-5-dehydroxylmethyl)-\b-cyclodextrins and
 their selective recognition ability utilizing multiple hydrogen bonds
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00517J
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_sum            'C145 H227.5 N12.5 O91'
_chemical_formula_weight         3601.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.676(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.1191(11)
_cell_length_b                   29.2535(18)
_cell_length_c                   19.9019(13)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.422
_cell_measurement_theta_min      2.326
_cell_volume                     9962.5(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            280570
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        21.490
_diffrn_reflns_theta_max         21.490
_diffrn_reflns_theta_min         1.024
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
 SADABS-2014/4 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3826
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Flack x determined using 9069 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1982
_refine_ls_number_reflns         22874
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      2.323
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.1111
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2853
_refine_ls_wR_factor_ref         0.2905
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                20889
_reflns_number_total             22874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00517j2.cif
_cod_data_source_block           042b_a
_cod_original_formula_sum        'C145 H227.50 N12.50 O91'
_cod_database_code               7123013
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              85191