Selective gas adsorption in microporous metal-organic frameworks incorporating urotropine basic sites: an experimental and theoretical study
S. A. Sapchenko; D. N. Dybtsev; D. G. Samsonenko; R. V. Belosludov; V. R. Belosludov; Y. Kawazoe; M. Schroder; V. P. Fedin; Chem.Commun. 51 (2015) 13918–; doi:10.1039/C5cc05779E

data_7117721
_publ_section_title
;
 Selective gas adsorption in microporous metal-organic frameworks
 incorporating urotropine basic sites: an experimental and theoretical
 study
;
_journal_name_full               Chem.Commun.
_journal_page_first              13918
_journal_paper_doi               10.1039/C5cc05779E
_journal_volume                  51
_journal_year                    2015
_chemical_formula_structural
'(Zn11 (H2 O)2 (C6 H12 N4)4 (C14 H8 O4)11) . 7(C3 H7 N O)'
_chemical_formula_sum            'C199 H189 N23 O53 Zn11'
_chemical_formula_weight         4469.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-13 deposited with the CCDC.
2015-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.845(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.018(1)
_cell_length_b                   20.783(1)
_cell_length_c                   37.062(1)
_cell_measurement_reflns_used    21523
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      35.25
_cell_measurement_theta_min      1.71
_cell_volume                     16899.0(12)
_computing_cell_refinement       'DENZO (Z. Otwinowski & W. Minor, 1997)'
_computing_data_collection       'ADSC Quantum software'
_computing_data_reduction        'HKL2000 (Z. Otwinowski & W. Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker-AXS, 2004)'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 19.5
_diffrn_measured_fraction_theta_full 0.830
_diffrn_measured_fraction_theta_max 0.791
_diffrn_measurement_device_type  'ADSC Quantum 210'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'Double Crystal Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.90000
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            94135
_diffrn_reflns_theta_full        34.50
_diffrn_reflns_theta_max         35.25
_diffrn_reflns_theta_min         1.71
_diffrn_source                   synchrotron
_diffrn_source_type              'PAL Beamline 2D'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.8871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Z. Otwinowski & W. Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4596
_exptl_crystal_preparation       'gas sorption'
_exptl_crystal_recrystallization_method
'crystallization during the solvothermal reaction'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.572
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00245(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1313
_refine_ls_number_reflns         29546
_refine_ls_number_restraints     350
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2235
_refine_ls_wR_factor_ref         0.2339
_reflns_number_gt                21523
_reflns_number_total             29546
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5cc05779e2.cif
_cod_data_source_block           sas274c
_cod_database_code               7117721