Selective carbon dioxide sorption by a new breathing three-dimensional Zn-MOF with Lewis basic nitrogen-rich channels.
Kim, Hyun-Chul; Huh, Seong; Lee, Do Nam; Kim, Youngmee; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4820–4826; doi:10.1039/C7DT04134A

data_1549026
_publ_section_title
;
 Selective carbon dioxide sorption by a new breathing three-dimensional
 Zn-MOF with Lewis basic nitrogen-rich channels.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4820
_journal_page_last               4826
_journal_paper_doi               10.1039/C7DT04134A
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C96 H64 N12 O16 Zn4, 0.5(C96 H66 N12 O16 Zn4), 5(C3 H7 N O)'
_chemical_formula_sum            'C159 H132 N23 O29 Zn6'
_chemical_formula_weight         3221.09
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-26 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.435(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.255(3)
_cell_length_b                   18.811(4)
_cell_length_c                   23.568(4)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.34
_cell_volume                     7194(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2006
_diffrn_reflns_av_unetI/netI     0.0889
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            210973
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_min         1.386
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       plate
_exptl_crystal_F_000             3318
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.718
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1076
_refine_ls_number_reflns         15280
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1803
_refine_ls_R_factor_gt           0.1197
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+52.4707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9476
_reflns_number_total             15280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04134a2.cif
_cod_data_source_block           zn-mof1
_cod_depositor_comments
'Adding full bibliography for 1549026--1549027.cif.'
_cod_database_code               1549026
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.674
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C84A, C84B}
3. Restrained distances
 C72-C69
 1.51 with sigma of 0.02
 C74-C73
 1.51 with sigma of 0.02
 C73-C72
 1.54 with sigma of 0.02
 C68-C72 \\sim C70-C72
 with sigma of 0.02
 C75-C73 \\sim C78-C73
 with sigma of 0.02
4. Restrained planarity
 N9, C67, C68, C69, C70, C71, C72
 with sigma of 0.1
 C73, C74, C75, C76, C77, C78, N10
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq,
Uanis(C74) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(N9) \\sim Ueq:
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C84A) = Uanis(C84B)
6. Rigid body (RIGU) restrains
 N9, N10, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, C44, C48, C47, C42, C45, C46, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C84B, N12A, C82A, C83A, O14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{O13, N11, C79, C80, C81} sigma for 1-2: 0.02, 1-3: 0.04
as
{O16, N13, C88, C89, C90}
8. Others
 Fixed Sof: N9(0.5) C71(0.5) H71(0.5) C70(0.5) H70(0.5) C69(0.5) C68(0.5)
 H68(0.5) C67(0.5) H67(0.5) C72(0.5) H72A(0.5) H72B(0.5) C73(0.5) H73A(0.5)
 H73B(0.5) N10(0.5) H10A(0.5) C77(0.5) H77(0.5) C78(0.5) H78(0.5) C74(0.5)
 C75(0.5) H75(0.5) C76(0.5) H76(0.5) O14A(0.5) N12A(0.5) C82A(0.5) H82A(0.5)
 C83A(0.5) H83A(0.5) H83B(0.5) H83C(0.5) C84A(0.5) H84A(0.5) H84B(0.5)
 H84C(0.5) O14B(0.5) N12B(0.5) C82B(0.5) H82B(0.5) C83B(0.5) H83D(0.5)
 H83E(0.5) H83F(0.5) C84B(0.5) H84D(0.5) H84E(0.5) H84F(0.5) O15(0.25)
 N14(0.25) C85(0.25) H85(0.25) C86(0.25) H86A(0.25) H86B(0.25) H86C(0.25)
 C87(0.25) H87A(0.25) H87B(0.25) H87C(0.25) O16(0.25) N13(0.25) C88(0.25)
 H88(0.25) C89(0.25) H89A(0.25) H89B(0.25) H89C(0.25) C90(0.25) H90A(0.25)
 H90B(0.25) H90C(0.25)
9.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C43(H43A,H43B), C72(H72A,H72B), C73(H73A,H73B)
9.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C17(H17), C21(H21), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28),
  C31(H31), C32(H32), C33(H33), C35(H35), C37(H37), C38(H38), C40(H40),
 C41(H41), C45(H45), C46(H46), C47(H47), C48(H48), C51(H51), C53(H53), C54(H54),
  C55(H55), C57(H57), C58(H58), C61(H61), C63(H63), C64(H64), C65(H65),
 C71(H71), C70(H70), C68(H68), C67(H67), N10(H10A), C77(H77), C78(H78),
 C75(H75), C76(H76), C79(H79), C82A(H82A), C82B(H82B), C85(H85), C88(H88)
9.c Fitted hexagon refined as free rotating group:
 N9(C71,C70,C69,C68,C67), N10(C77,C78,C74,C75,C76)
9.d Idealised Me refined with riding coordinates:
 C84A(H84A,H84B,H84C), C84B(H84D,H84E,H84F), C89(H89A,H89B,H89C), C90(H90A,
 H90B,H90C)
9.e Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C83A(H83A,H83B,H83C), C83B(H83D,
 H83E,H83F), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C)
;
_olex2_submission_special_instructions 'No special instructions were received'