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_4344840
_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 O24), 4(Cl0.75 O3)'
_chemical_formula_sum            'C36 H24 Cl4 Cu4 N12 O24'
_chemical_formula_weight         1404.63
_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     direct
_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                   14.2066(2)
_cell_length_b                   14.2066(2)
_cell_length_c                   19.8137(4)
_cell_measurement_temperature    150
_cell_volume                     3998.95(11)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5728
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.912
_diffrn_reflns_theta_min         3.829
_exptl_absorpt_coefficient_mu    2.974
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1400
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.861
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1192
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0966
_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^)+(0.2000P)^2^+37.8050P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2861
_refine_ls_wR_factor_ref         0.2886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1150
_reflns_number_total             1192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02316_si_002.cif
_cod_data_source_block           FJU-14-ClO4
_cod_original_cell_volume        3998.92(14)
_cod_database_code               4344840
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N1, C3}
3. Restrained distances
 Cl2-O4 = Cl2-O3
 1.326 with sigma of 0.02
 H6-H4
 1.8 with sigma of 0.02
 H6-H4
 1.9 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.1A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O4) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C3) = Uanis(N1)
Uanis(N1) = Uanis(C3)
Uanis(O4) = Uanis(Cl2) = Uanis(O3)
Uanis(N2) = Uanis(O1)
5. Others
 Fixed Sof: N2(0.5) N1(0.25) C1(0.25) C5(0.25) C2(0.5) H2(0.5) C4(0.5) H4(0.5)
 O1(0.5) C3(0.25) Cl2(0.1875) O3(0.375) O4(0.375)
6.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C4(H4)
;
_shelx_res_checksum              38740
_shelx_hkl_checksum              96841
_shelx_fab_checksum              29400
_olex2_submission_special_instructions 'No special instructions were received'