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_4344841
_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 O20), 4(B0.75 F3), 2(O)'
_chemical_formula_sum            'C36 H24 B3 Cl Cu4 F12 N12 O12'
_chemical_formula_weight         1366.71
_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
_audit_creation_date             2015-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1125(5)
_cell_length_b                   14.1125(5)
_cell_length_c                   19.8583(7)
_cell_measurement_temperature    150
_cell_volume                     3955.0(2)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_laue_measured_fraction_full 0.986
_diffrn_reflns_laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4307
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.994
_diffrn_reflns_theta_min         3.843
_exptl_absorpt_coefficient_mu    2.184
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.722
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1139
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1380P)^2^+1.8621P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                889
_reflns_number_total             1139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02316_si_002.cif
_cod_data_source_block           FJU-14-BF4
_cod_original_cell_volume        3955.1(3)
_cod_database_code               4344841
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N4, C18A}
3. Restrained distances
 F2-B1 = F1-B1
 1.42 with sigma of 0.02
 Cu1-OW
 2.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(OWA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N4) = Uanis(C18A)
Uanis(C2) = Uanis(C3) = Uanis(C1)
Uanis(OW) = Uanis(OWA)
5. Others
 Sof(OWA)=0.25*(1-FVAR(2))
 Sof(OW)=0.25*FVAR(2)
 Fixed Sof: N2(0.5) N4(0.25) C3(0.5) H3(0.5) C6(0.25) F1(0.375) C5(0.5)
 H5(0.5) C2(0.25) F2(0.375) B1(0.1875) O1(0.5) C18A(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5)
;
_shelx_res_checksum              57484
_shelx_hkl_checksum              31115
_shelx_fab_checksum              68409
_olex2_submission_special_instructions 'No special instructions were received'