Distinctive Three-Step Hysteretic Sorption of Ethane with In-situ Crystallographic Visualization of the Pore Forms in a Soft Porous Crystal.
Lama, Prem; Barbour, Leonard J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10352

data_4126905
_publ_section_title
;
 Distinctive Three-Step Hysteretic Sorption of Ethane with In-situ
 Crystallographic Visualization of the Pore Forms in a Soft Porous
 Crystal.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10352
_journal_year                    2017
_chemical_formula_moiety         '0.5(C40 H24 N12 O16 Zn6)'
_chemical_formula_sum            'C20 H12 N6 O8 Zn3'
_chemical_formula_weight         660.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.063(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8288(4)
_cell_length_b                   19.6384(9)
_cell_length_c                   8.0916(4)
_cell_measurement_reflns_used    523
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.16
_cell_measurement_theta_min      2.07
_cell_volume                     1270.85(11)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex DUO CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            39062
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.074
_exptl_absorpt_coefficient_mu    2.863
_exptl_absorpt_correction_T_max  25.000
_exptl_absorpt_correction_T_min  2.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+2.0905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1954
_reflns_number_total             2235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1eI_squeeze.cif
_cod_data_source_block           1eI_squeeze
_cod_original_cell_volume        1270.85(10)
_cod_database_code               4126905
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.598
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C9A(0.6) H9A(0.6) C9B(0.4) H9B(0.4) C10A(0.6) H10A(0.6) C10B(0.4)
 H10B(0.4)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9A(H9A), C9B(H9B), C10A(H10A), C10B(H10B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'