#------------------------------------------------------------------------------
#$Date: 2016-02-04 03:23:23 +0200 (Thu, 04 Feb 2016) $
#$Revision: 175668 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/48/4344843.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4344843
loop_
_publ_author_name
'Ye, Yingxiang'
'Xiong, Shunshun'
'Wu, Xiaonan'
'Zhang, Liuqin'
'Li, Ziyin'
'Wang, Lihua'
'Ma, Xiuling'
'Chen, Qian-Huo'
'Zhang, Zhangjing'
'Xiang, Shengchang'
_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       'ω 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/[σ²(Fo²)+(0.1830P)²+20.4060P]
 where P=(Fo²+2Fc²)/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 > 2σ(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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'x, -y, -z'
'-x, -y, z'
'-y, -x, -z'
'y, x, -z'
'y, -x, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'-x, y, z'
'x, y, -z'
'y, x, z'
'-y, -x, z'
'-y, x, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.18067(9) 0.0000 0.0000 0.0229(5) Uani 1 4 d S T P . .
Cl1 Cl 0.0000 0.0000 0.0000 0.0454(13) Uani 1 16 d S T P A .
N2 N 0.1737(13) -0.1059(15) -0.0681(11) 0.036(4) Uani 0.5 1 d . . . A 1
N1 N 0.1970(4) -0.1970(4) -0.1594(4) 0.0425(16) Uani 0.5 2 d S T P A 1
C2 C 0.3085(6) -0.1915(6) -0.2500 0.094(4) Uani 1 2 d S TU P . .
H2 H 0.3564 -0.1436 -0.2500 0.112 Uiso 1 2 calc RS T P B 2
C6 C 0.2221(8) -0.1144(8) -0.1238(5) 0.040(2) Uani 0.5 1 d . . . A 1
H6 H 0.2688 -0.0700 -0.1384 0.048 Uiso 0.5 1 calc R . . A 1
F1 F 0.4198(9) 0.0000 -0.1530(9) 0.128(5) Uani 0.75 2 d S T P . .
C5 C 0.1637(7) 0.1637(7) 0.0968(7) 0.029(3) Uani 0.5 2 d S TU P A 2
C3 C 0.2241(9) -0.2241(9) -0.2218(6) 0.046(4) Uani 0.5 2 d S T P A 1
B1 B 0.5000 0.0000 -0.183(2) 0.113(14) Uani 0.75 4 d S T P . .
F2 F 0.5000 -0.0748(16) -0.2370(19) 0.239(16) Uani 0.75 2 d S T P . .
C1 C 0.2824(14) -0.1662(14) -0.1880(9) 0.087(5) Uani 0.5 1 d . U . A 2
H1 H 0.3232 -0.1259 -0.1626 0.104 Uiso 0.5 1 calc R . . A 2
O1 O 0.2023(10) 0.0901(10) 0.0735(8) 0.032(3) Uani 0.5 1 d . . . A 2
C4 C 0.1970(4) -0.1970(4) -0.1594(4) 0.0425(16) Uani 0.5 2 d S TU P A 2
Ow O 0.3563(14) -0.0320(13) 0.0000 0.084(6) Uani 0.5 2 d S T P C 1
C7 C 0.5000 0.0000 0.0000 0.020(6) Uani 0.1744 8 d DS TU P . .
O4 O 0.5000 0.0000 -0.0587(10) 0.020(6) Uani 0.0872 4 d DS TU P D 1
C8 C 0.0000 0.0000 -0.215(4) 0.11(2) Uani 0.2925 8 d DS T P . .
O3 O 0.0939(14) 0.0000 -0.216(4) 0.11(2) Uani 0.1463 2 d DS T P E 1
O4A O 0.414(4) 0.0000 0.0000 0.020(6) Uani 0.0872 4 d S TU P D 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Cu1 Cl1 87.2(5) . .
N2 Cu1 Cl1 87.2(5) 20 .
N2 Cu1 Cl1 87.2(5) 3 .
N2 Cu1 Cl1 87.2(5) 24 .
N2 Cu1 N2 174.4(10) . 3
N2 Cu1 N2 95.0(13) . 24
N2 Cu1 N2 174.4(10) 24 20
N2 Cu1 N2 84.7(12) . 20
N2 Cu1 N2 84.7(12) 3 24
N2 Cu1 N2 95.0(13) 3 20
O1 Cu1 Cl1 98.9(4) . .
O1 Cu1 Cl1 98.9(4) 20 .
O1 Cu1 Cl1 98.9(4) 3 .
O1 Cu1 Cl1 98.9(4) 24 .
O1 Cu1 O1 80.4(8) . 24
O1 Cu1 O1 162.2(8) . 3
O1 Cu1 O1 162.2(8) 24 20
O1 Cu1 O1 96.9(9) 3 24
O1 Cu1 O1 96.9(9) . 20
O1 Cu1 O1 80.4(8) 3 20
Cu1 Cl1 Cu1 180.0 . 17
Cu1 Cl1 Cu1 90.0 18 17
Cu1 Cl1 Cu1 180.0 18 2
Cu1 Cl1 Cu1 90.0 . 18
Cu1 Cl1 Cu1 90.0 . 2
Cu1 Cl1 Cu1 90.0 17 2
N2 N2 Cu1 123.8(4) 22 .
C6 N2 Cu1 127.9(11) . .
C6 N2 N2 107.6(9) . 22
C6 N1 C6 99.2(9) 22 .
C3 N1 C6 128.7(5) . .
C3 N1 C6 128.7(5) . 22
C3 C2 C3 66.5(10) 25_544 .
C1 C2 C1 179(2) . 14_544
N2 C6 N1 112.0(11) . .
O1 C5 O1 125.0(16) 21 .
O1 C5 C4 117.2(8) . 3
O1 C5 C4 117.2(8) 21 3
N1 C3 C2 121.2(5) . 25_544
N1 C3 C2 121.2(5) . .
N1 C3 C3 161(2) . 25_544
C2 C3 C2 113.5(10) 25_544 .
C2 C3 C3 56.7(5) 25_544 25_544
C2 C3 C3 56.7(5) . 25_544
F1 B1 F1 124(4) 19_655 .
F1 B1 F2 109.7(10) 19_655 4_655
F1 B1 F2 109.7(10) . 4_655
F1 B1 F2 84.7(13) 19_655 13_554
F1 B1 F2 109.7(10) 19_655 .
F1 B1 F2 84.7(13) . 26_554
F1 B1 F2 151(3) 19_655 26_554
F1 B1 F2 109.7(10) . .
F1 B1 F2 151(3) . 13_554
F2 B1 F2 53.3(17) . 26_554
F2 B1 F2 53.3(17) . 13_554
F2 B1 F2 89(4) 4_655 .
F2 B1 F2 67(2) 26_554 13_554
F2 B1 F2 53.3(17) 4_655 26_554
F2 B1 F2 53.3(17) 4_655 13_554
B1 F2 B1 102(3) . 26_554
B1 F2 F2 76.7(16) . 13_554
B1 F2 F2 76.7(16) . 26_554
F2 F2 B1 50.1(19) 26_554 26_554
F2 F2 B1 50.1(19) 13_554 26_554
F2 F2 F2 83.8(15) 13_554 26_554
C5 O1 Cu1 137.8(10) . .
O4 C7 O4 180.0 3 .
O4A C7 O4A 180.0 17_655 .
O3 C8 O3 89.999(13) . 2
O3 C8 O3 89.999(16) 4 2
O3 C8 O3 89.999(14) 4 7
O3 C8 O3 89.999(15) . 7
O3 C8 O3 179.4(18) 4 .
O3 C8 O3 179.4(18) 2 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cl1 2.5338(12) .
Cu1 N2 2.01(2) 3
Cu1 N2 2.01(2) 24
Cu1 N2 2.01(2) .
Cu1 N2 2.01(2) 20
Cu1 O1 1.960(16) 24
Cu1 O1 1.960(16) 3
Cu1 O1 1.960(16) .
Cu1 O1 1.960(16) 20
Cl1 Cu1 2.5338(12) 18
Cl1 Cu1 2.5338(12) 2
Cl1 Cu1 2.5338(12) 17
N2 N2 1.35(3) 22
N2 C6 1.31(2) .
N1 C6 1.403(11) 22
N1 C6 1.403(11) .
N1 C3 1.357(13) .
C2 C3 1.388(12) .
C2 C3 1.388(12) 25_544
C2 C1 1.338(16) .
C2 C1 1.338(16) 14_544
F1 B1 1.27(2) .
C5 O1 1.254(15) 21
C5 O1 1.254(15) .
C5 C4 1.411(15) 3
C3 C2 1.388(12) 25_544
C3 C3 1.52(2) 25_544
B1 F1 1.27(2) 19_655
B1 F2 1.91(5) 13_554
B1 F2 1.50(4) 4_655
B1 F2 1.91(5) 26_554
B1 F2 1.50(4) .
F2 B1 1.91(5) 26_554
F2 F2 1.57(5) 26_554
F2 F2 1.57(5) 13_554
Ow Ow 0.90(4) 3
C7 O4 1.17(2) .
C7 O4 1.17(2) 3
C7 O4A 1.20(6) 17_655
C7 O4A 1.20(6) .
C8 O3 1.317(19) 4
C8 O3 1.317(19) .
C8 O3 1.317(19) 2
C8 O3 1.317(19) 7
