Microporous Metal-Organic Framework Stabilized by Balanced Multiple Host-Couteranion Hydrogen-Bonding Interactions for High-Density CO2 Capture at Ambient Conditions.
Ye, Yingxiang; Xiong, Shunshun; Wu, Xiaonan; Zhang, Liuqin; Li, Ziyin; Wang, Lihua; Ma, Xiuling; Chen, Qian-Huo; Zhang, Zhangjing; Xiang, Shengchang; Inorganic chemistry 55 (2015) 292–; doi:10.1021/acs.inorgchem.5b02316

data_4344843
_publ_section_title
;
 Microporous Metal-Organic Framework Stabilized by Balanced Multiple
 Host-Couteranion Hydrogen-Bonding Interactions for High-Density CO2
 Capture at Ambient Conditions.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              292
_journal_paper_doi               10.1021/acs.inorgchem.5b02316
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety
'0.5(C72 H48 Cl2 Cu8 N24 O16), 4(B0.75 F3), 2(Ow), 0.23(C4 O8)'
_chemical_formula_sum            'C36.94 H24 B3 Cl Cu4 F12 N12 O13.87'
_chemical_formula_weight         1407.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0241(7)
_cell_length_b                   14.0241(7)
_cell_length_c                   19.9373(11)
_cell_measurement_reflns_used    1801
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.2870
_cell_measurement_theta_min      3.7950
_cell_volume                     3921.2(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -73.00   35.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.8249   77.0000 -150.0000 108

  2 omega    8.00  117.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.8249   77.0000  150.0000 109

  3 omega   74.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   77.0000  150.0000 104

  4 omega   74.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   77.0000 -180.0000 104

  5 omega   74.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   77.0000 -120.0000 104

  6 omega   74.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   77.0000 -150.0000 56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0518793000
_diffrn_orient_matrix_UB_12      0.0806185000
_diffrn_orient_matrix_UB_13      -0.0377844000
_diffrn_orient_matrix_UB_21      -0.0162327500
_diffrn_orient_matrix_UB_22      0.0672687500
_diffrn_orient_matrix_UB_23      0.0599916500
_diffrn_orient_matrix_UB_31      0.0955666500
_diffrn_orient_matrix_UB_32      -0.0321588500
_diffrn_orient_matrix_UB_33      0.0306278500
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6882
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.043
_diffrn_reflns_theta_min         3.854
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1393
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.939
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1163
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0936
_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^)+(0.1830P)^2^+20.4060P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2499
_refine_ls_wR_factor_ref         0.2703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                964
_reflns_number_total             1163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02316_si_002.cif
_cod_data_source_block           FJU-14-BF4-CO2
_cod_database_code               4344843
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         ' C N O H F B Cl Cu'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N1, C4}
3. Restrained distances
 O4_$4-C7
 1.16 with sigma of 0.02
 C8-O3
 1.314 with sigma of 0.02
4. Restrained planarity
 C8, O3_$3, O3_$2, O3, O3_$1
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C7 \\sim O4A \\sim O4: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C7) = Uanis(O4)
Uanis(C7) = Uanis(O4A)
Uanis(C8) = Uanis(O3)
Uanis(N1) = Uanis(C4)
6. Others
 Fixed Sof: N2(0.5) N1(0.25) C6(0.5) H6(0.5) F1(0.375) C5(0.25) C3(0.25)
 B1(0.1875) F2(0.375) C1(0.5) H1(0.5) O1(0.5) C4(0.25) Ow(0.25) C7(0.0218)
 O4(0.0218) C8(0.03657) O3(0.07314) O4A(0.0218)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C1(H1)
;
_shelx_res_checksum              80199
_shelx_hkl_checksum              10445
_olex2_submission_special_instructions 'No special instructions were received'