Water adsorption in porous organic crystals of adamantane-bearing macrocycles
Tominaga, Masahide; Hyodo, Tadashi; Mizuno, Kosuke; Kawahata, Masatoshi; Yamaguchi, Kentaro; CrystEngComm  (2022) –; doi:10.1039/D2CE01030E

data_7245459
_publ_section_title
;
 Water adsorption in porous organic crystals of adamantane-bearing
 macrocycles
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01030E
_journal_year                    2022
_chemical_formula_sum            'C54.31 H48.62 Cl8.62 N4 O4'
_chemical_formula_weight         1126.80
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-14 deposited with the CCDC.	2022-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.313(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3935(11)
_cell_length_b                   7.0220(5)
_cell_length_c                   23.5881(15)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.44
_cell_measurement_theta_min      3.61
_cell_volume                     2631.1(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (H\"ubschle et al., 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34786
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.692
_diffrn_reflns_theta_min         2.969
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    4.606
_exptl_absorpt_correction_T_max  0.9403
_exptl_absorpt_correction_T_min  0.8968
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.972
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5374
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1161P)^2^+3.5081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.1944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5275
_reflns_number_total             5374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01030e2.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7245459
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.459
_shelx_estimated_absorpt_t_max   0.491
_shelx_res_checksum              22360
_shelx_hkl_checksum              87025