Stepwise and hysteretic sorption of CO2 in polycatenated metal‒organic frameworks
Chen, Di-Ming; Zhang, Xue-Jing; CrystEngComm 21 (2019) 4696–; doi:10.1039/C9CE00760A

data_7233028
_publ_section_title
;
 Stepwise and hysteretic sorption of CO2 in polycatenated metal--organic
 frameworks
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4696
_journal_paper_doi               10.1039/C9CE00760A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C62 H48 N6 O10 Zn2'
_chemical_formula_sum            'C62 H48 N6 O10 Zn2'
_chemical_formula_weight         1167.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc13w369
_audit_creation_date             2014-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-02-17 deposited with the CCDC.    2019-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.725(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.1240(12)
_cell_length_b                   17.0584(5)
_cell_length_c                   30.6102(13)
_cell_measurement_reflns_used    5978
_cell_measurement_temperature    129.90(14)
_cell_measurement_theta_max      28.3970
_cell_measurement_theta_min      3.2390
_cell_volume                     12010.1(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      129.90(14)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -20.00   54.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000 -180.0000 74

  2 omega  -10.00   85.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000  -30.0000 95

  3 omega  -38.00   10.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -19.0000 -150.0000 48
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0221767000
_diffrn_orient_matrix_UB_12      -0.0008280000
_diffrn_orient_matrix_UB_13      -0.0234120000
_diffrn_orient_matrix_UB_21      -0.0006048000
_diffrn_orient_matrix_UB_22      -0.0415393000
_diffrn_orient_matrix_UB_23      0.0009864000
_diffrn_orient_matrix_UB_31      -0.0214516000
_diffrn_orient_matrix_UB_32      0.0021437000
_diffrn_orient_matrix_UB_33      0.0095078000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22446
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4816
_platon_squeeze_details
;
;
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         10540
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                7389
_reflns_number_total             10540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ce00760a2.cif
_cod_data_source_block           2_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7233027--7233028.cif.'
_cod_original_cell_volume        12010.1(8)
_cod_database_code               7233028
_chemical_oxdiff_formula         'C Zn'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O37-H37
 0.85 with sigma of 0.01
 O39-H39
 0.85 with sigma of 0.01
 C12-H37
 1.898948 with sigma of 0.02
 Zn6-H37
 2.843748 with sigma of 0.02
 C300-H39
 1.885738 with sigma of 0.02
 Zn2-H39
 2.712923 with sigma of 0.02
3. Rigid bond restraints
 O37, C12, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O37: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O37: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O37 \\sim C12 \\sim C6: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5.a Secondary CH2 refined with riding coordinates:
 C300(H30a,H30b), C12(H12a,H12b)
5.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C45(H45), C48(H48), C68(H68), C87(H87), C89(H89), C92(H92),
 C95(H95), C122(H122), C128(H128), C129(H129), C140(H140), C143(H143),
 C150(H150), C154(H154), C161(H161), C166(H166), C171(H171), C176(H176),
 C194(H194), C195(H195), C209(H209), C211(H211), C217(H217), C245(H245),
 C248(H248), C250(H250), C251(H251), C254(H254), C272(H272), C282(H282),
 C287(H287), C289(H289), C295(H295), C302(H302), C322(H322)
5.c Idealised Me refined as rotating group:
 C333(H33a,H33b,H33c), C6(H6a,H6b,H6c)
;
_olex2_submission_special_instructions 'No special instructions were received'