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_4126907
_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         'C20 H12 N6 O8 Zn3'
_chemical_formula_sum            'C20 H12 N6 O8 Zn3'
_chemical_formula_weight         660.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                115.321(10)
_cell_angle_beta                 97.689(9)
_cell_angle_gamma                97.641(9)
_cell_formula_units_Z            1
_cell_length_a                   9.102(3)
_cell_length_b                   10.739(4)
_cell_length_c                   11.209(4)
_cell_measurement_reflns_used    5042
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.20
_cell_volume                     959.1(6)
_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 D8 venture PHOTON II CPAD'
_diffrn_measurement_method       '\f \ch and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_av_unetI/netI     0.1754
_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       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6746
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.057
_exptl_absorpt_coefficient_mu    1.897
_exptl_absorpt_correction_T_max  24.997
_exptl_absorpt_correction_T_min  2.057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0890
_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^)+(0.0852P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1726
_reflns_number_total             3375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1eII_squeeze.cif
_cod_data_source_block           1eII_squeeze
_cod_database_code               4126907
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.680
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9A) \\sim Ueq, Uanis(C9B) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.01
Uanis(C10B) \\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.01
3. Others
 Fixed Sof: C9A(0.5) H9A(0.5) C9B(0.5) H9B(0.5) C10A(0.6) H10A(0.6) C10B(0.4)
 H10B(0.4)
 Fixed X: C10B(0.936319)
 Fixed Y: C10B(0.18415)
 Fixed Z: C10B(0.276419)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9A(H9A), C9B(H9B), C10A(H10A), C10B(H10B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'