#------------------------------------------------------------------------------
#$Date: 2019-11-25 23:20:35 +0200 (Mon, 25 Nov 2019) $
#$Revision: 242040 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/19/4131998.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_4131998
loop_
_publ_author_name
'Bao, Zongbi'
'Xie, Danyan'
'Chang, Ganggang'
'Wu, Hui'
'Li, Liangying'
'Zhou, Wei'
'Wang, Hailong'
'Zhang, Zhiguo'
'Xing, Huabin'
'Yang, Qiwei'
'Zaworotko, Michael J.'
'Ren, Qilong'
'Chen, Banglin'
_publ_section_title
;
 Fine Tuning and Specific Binding Sites with a Porous Hydrogen-Bonded
 Metal-Complex Framework for Gas Selective Separations.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4596
_journal_page_last               4603
_journal_paper_doi               10.1021/jacs.7b13706
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C20 H24 Cu2 N20 O2, 2(F6 Si)'
_chemical_formula_sum            'C20 H24 Cu2 F12 N20 O2 Si2'
_chemical_formula_weight         987.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9982(8)
_cell_length_b                   11.0287(5)
_cell_length_c                   21.3180(11)
_cell_measurement_reflns_used    3475
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1059
_cell_measurement_theta_min      2.9095
_cell_volume                     3996.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0187031000
_diffrn_orient_matrix_UB_12      -0.0267706000
_diffrn_orient_matrix_UB_13      -0.0263155000
_diffrn_orient_matrix_UB_21      -0.0124493000
_diffrn_orient_matrix_UB_22      -0.0491517000
_diffrn_orient_matrix_UB_23      0.0190265000
_diffrn_orient_matrix_UB_31      -0.0351489000
_diffrn_orient_matrix_UB_32      0.0317051000
_diffrn_orient_matrix_UB_33      0.0072654000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12448
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_platon_squeeze_details
;
;
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0774P)²+8.8562P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                1581
_reflns_number_total             1941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b13706_si_002.cif
_cod_data_source_block           160111_xdy_mpmf
_cod_database_code               4131998
_chemical_oxdiff_formula         'C10 H10 N2 O8 F1 Cu1'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
3.a Rotating group:
 O1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C4(H4)
3.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z+1/2'
3 'x, -y, -z'
4 '-x, y, -z+1/2'
5 'x+1/2, y+1/2, z'
6 '-x+1/2, -y+1/2, z+1/2'
7 'x+1/2, -y+1/2, -z'
8 '-x+1/2, y+1/2, -z+1/2'
9 '-x, -y, -z'
10 'x, y, -z-1/2'
11 '-x, y, z'
12 'x, -y, z-1/2'
13 '-x+1/2, -y+1/2, -z'
14 'x+1/2, y+1/2, -z-1/2'
15 '-x+1/2, y+1/2, z'
16 '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_calc_flag
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.06778(5) 0.44005(3) 0.0270(2) Uani 1 d 2 S T P
O1 O 0.5000 0.1599(4) 0.35002(19) 0.0457(10) Uani 1 d 2 S T P
H1A H 0.5203 0.2323 0.3533 0.069 Uiso 0.50 d 1 GR . .
H1B H 0.4522 0.1673 0.3356 0.069 Uiso 0.50 d 1 GR . .
N1 N 0.58268(18) -0.0574(3) 0.41995(16) 0.0308(7) Uani 1 d 1 . . .
N2 N 0.6647(2) -0.1735(3) 0.36619(17) 0.0421(9) Uani 1 d 1 . . .
H2 H 0.6933 -0.2002 0.3359 0.050 Uiso 1 calc 1 R . .
N3 N 0.58236(17) -0.1714(3) 0.51767(15) 0.0304(7) Uani 1 d 1 . . .
N4 N 0.6606(2) -0.3493(3) 0.51373(18) 0.0434(9) Uani 1 d 1 . . .
N5 N 0.7226(3) -0.4192(3) 0.4237(2) 0.0622(12) Uani 1 d 1 . . .
H5A H 0.7355 -0.4845 0.4432 0.075 Uiso 1 calc 1 R . .
H5B H 0.7362 -0.4092 0.3852 0.075 Uiso 1 calc 1 R . .
C1 C 0.6196(2) -0.0757(4) 0.3658(2) 0.0378(9) Uani 1 d 1 . . .
H1 H 0.6144 -0.0249 0.3313 0.045 Uiso 1 calc 1 R . .
C2 C 0.6565(2) -0.2242(4) 0.4256(2) 0.0399(10) Uani 1 d 1 . . .
C3 C 0.6063(2) -0.1514(3) 0.45844(19) 0.0310(8) Uani 1 d 1 . . .
C4 C 0.6139(3) -0.2716(4) 0.5425(2) 0.0397(10) Uani 1 d 1 . . .
H4 H 0.6017 -0.2881 0.5842 0.048 Uiso 1 calc 1 R . .
C5 C 0.6813(2) -0.3325(4) 0.4536(2) 0.0460(11) Uani 1 d 1 . . .
Si1 Si 0.81741(11) -0.28511(19) 0.2500 0.0496(5) Uani 1 d 2 S T P
F1 F 0.7436(3) -0.1850(4) 0.2500 0.0795(14) Uani 1 d 2 S T P
F2 F 0.8620(4) -0.2112(5) 0.3042(3) 0.171(3) Uani 1 d 1 . . .
F3 F 0.7711(3) -0.3598(5) 0.3047(3) 0.173(3) Uani 1 d 1 . . .
F4 F 0.8898(3) -0.3894(5) 0.2500 0.0811(14) Uani 1 d 2 S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
O1 Cu1 Cu1 177.58(13) . 9_656
N1 Cu1 Cu1 80.66(10) 11_655 9_656
N1 Cu1 Cu1 80.66(10) . 9_656
N1 Cu1 O1 97.62(13) 11_655 .
N1 Cu1 O1 97.62(13) . .
N1 Cu1 N1 88.39(17) . 11_655
N1 Cu1 N3 89.94(12) . 3_556
N1 Cu1 N3 164.92(13) 11_655 3_556
N1 Cu1 N3 164.92(13) . 9_656
N1 Cu1 N3 89.94(12) 11_655 9_656
N3 Cu1 Cu1 84.28(9) 3_556 9_656
N3 Cu1 Cu1 84.28(9) 9_656 9_656
N3 Cu1 O1 97.45(12) 9_656 .
N3 Cu1 O1 97.45(12) 3_556 .
N3 Cu1 N3 87.79(17) 3_556 9_656
Cu1 O1 H1A 111.0 . .
Cu1 O1 H1B 110.7 . .
H1A O1 H1B 108.1 . .
C1 N1 Cu1 128.2(3) . .
C1 N1 C3 105.3(3) . .
C3 N1 Cu1 126.1(3) . .
C1 N2 H2 127.0 . .
C1 N2 C2 105.9(3) . .
C2 N2 H2 127.0 . .
C3 N3 Cu1 122.4(2) . 9_656
C4 N3 Cu1 124.6(3) . 9_656
C4 N3 C3 112.7(3) . .
C4 N4 C5 120.8(4) . .
H5A N5 H5B 120.0 . .
C5 N5 H5A 120.0 . .
C5 N5 H5B 120.0 . .
N1 C1 H1 123.4 . .
N2 C1 N1 113.1(4) . .
N2 C1 H1 123.4 . .
N2 C2 C5 134.5(4) . .
C3 C2 N2 107.1(4) . .
C3 C2 C5 118.1(4) . .
N3 C3 N1 126.4(3) . .
N3 C3 C2 125.1(4) . .
C2 C3 N1 108.5(4) . .
N3 C4 H4 116.8 . .
N4 C4 N3 126.4(4) . .
N4 C4 H4 116.8 . .
N4 C5 N5 119.4(4) . .
N4 C5 C2 116.5(4) . .
N5 C5 C2 124.2(5) . .
F1 Si1 F4 178.3(3) . .
F2 Si1 F1 91.1(2) . .
F2 Si1 F1 91.1(2) 10_556 .
F2 Si1 F2 92.1(6) . 10_556
F2 Si1 F3 88.3(4) . .
F2 Si1 F3 179.3(3) 10_556 .
F2 Si1 F3 88.3(4) 10_556 10_556
F2 Si1 F3 179.3(3) . 10_556
F2 Si1 F4 90.1(2) 10_556 .
F2 Si1 F4 90.1(2) . .
F3 Si1 F1 88.3(2) . .
F3 Si1 F1 88.3(2) 10_556 .
F3 Si1 F3 91.3(5) 10_556 .
F3 Si1 F4 90.5(2) . .
F3 Si1 F4 90.5(2) 10_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu1 2.9612(12) 9_656
Cu1 O1 2.172(4) .
Cu1 N1 2.016(3) .
Cu1 N1 2.016(3) 11_655
Cu1 N3 2.019(3) 9_656
Cu1 N3 2.019(3) 3_556
O1 H1A 0.8721 .
O1 H1B 0.8723 .
N1 C1 1.329(5) .
N1 C3 1.381(5) .
N2 H2 0.8600 .
N2 C1 1.323(5) .
N2 C2 1.391(6) .
N3 Cu1 2.019(3) 9_656
N3 C3 1.345(5) .
N3 C4 1.338(5) .
N4 C4 1.320(5) .
N4 C5 1.343(6) .
N5 H5A 0.8600 .
N5 H5B 0.8600 .
N5 C5 1.346(6) .
C1 H1 0.9300 .
C2 C3 1.365(6) .
C2 C5 1.401(6) .
C4 H4 0.9300 .
Si1 F1 1.671(4) .
Si1 F2 1.604(5) .
Si1 F2 1.604(5) 10_556
Si1 F3 1.630(4) .
Si1 F3 1.630(4) 10_556
Si1 F4 1.684(4) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Cu1 Cu1 N1 C1 175.1(3) 9_656
Cu1 Cu1 N1 C3 2.9(3) 9_656
Cu1 N1 C1 N2 -173.3(3) .
Cu1 N1 C3 N3 -4.9(5) .
Cu1 N1 C3 C2 173.1(3) .
Cu1 N3 C3 N1 3.6(5) 9_656
Cu1 N3 C3 C2 -174.0(3) 9_656
Cu1 N3 C4 N4 171.4(3) 9_656
O1 Cu1 N1 C1 -3.2(3) .
O1 Cu1 N1 C3 -175.4(3) .
N1 Cu1 N1 C1 94.3(3) 11_655
N1 Cu1 N1 C3 -77.9(3) 11_655
N2 C2 C3 N1 0.7(4) .
N2 C2 C3 N3 178.7(3) .
N2 C2 C5 N4 -179.6(4) .
N2 C2 C5 N5 -0.7(8) .
N3 Cu1 N1 C1 -100.7(3) 3_556
N3 Cu1 N1 C1 178.0(4) 9_656
N3 Cu1 N1 C3 5.9(6) 9_656
N3 Cu1 N1 C3 87.1(3) 3_556
C1 N1 C3 N3 -178.5(4) .
C1 N1 C3 C2 -0.6(4) .
C1 N2 C2 C3 -0.6(4) .
C1 N2 C2 C5 172.2(5) .
C2 N2 C1 N1 0.3(5) .
C3 N1 C1 N2 0.2(5) .
C3 N3 C4 N4 -3.2(6) .
C3 C2 C5 N4 -7.4(6) .
C3 C2 C5 N5 171.5(4) .
C4 N3 C3 N1 178.3(4) .
C4 N3 C3 C2 0.7(5) .
C4 N4 C5 N5 -173.6(4) .
C4 N4 C5 C2 5.3(6) .
C5 N4 C4 N3 0.1(7) .
C5 C2 C3 N1 -173.5(4) .
C5 C2 C3 N3 4.5(6) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.002 484 66 ' '
2 0.500 0.500 0.733 484 66 ' '
