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#$Date: 2017-12-26 01:37:11 +0200 (Tue, 26 Dec 2017) $
#$Revision: 204514 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/69/4126904.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_4126904
loop_
_publ_author_name
'Lama, Prem'
'Barbour, Leonard J.'
_publ_section_title
;
 Distinctive Three-Step Hysteretic Sorption of Ethane with In-situ
 Crystallographic Visualization of the Pore Forms in a Soft Porous
 Crystal.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10352
_journal_year                    2017
_chemical_formula_sum            'C20 H12 N6 O8 Zn3'
_chemical_formula_weight         660.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                115.321(10)
_cell_angle_beta                 97.689(9)
_cell_angle_gamma                97.641(9)
_cell_formula_units_Z            1
_cell_length_a                   9.102(3)
_cell_length_b                   10.739(4)
_cell_length_c                   11.209(4)
_cell_measurement_reflns_used    5042
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.20
_cell_volume                     959.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 venture PHOTON II CPAD'
_diffrn_measurement_method       'φ \ch and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1077
_diffrn_reflns_av_unetI/netI     0.1757
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6742
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.057
_exptl_absorpt_coefficient_mu    1.897
_exptl_absorpt_correction_T_max  24.997
_exptl_absorpt_correction_T_min  2.057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.2122
_refine_ls_R_factor_gt           0.1207
_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)+(0.1648P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2959
_refine_ls_wR_factor_ref         0.3415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1724
_reflns_number_total             3373
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            1eII.cif
_cod_data_source_block           1eII
_cod_database_code               4126904
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_min   0.680
_shelx_estimated_absorpt_t_max   0.863
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Zn1 Zn 0.500000 0.000000 0.000000 0.0457(8) Uani 1 2 d S . P A .
Zn2 Zn 0.82012(18) -0.1154(2) -0.11772(18) 0.0428(6) Uani 1 1 d . . . . .
O1 O 0.5576(13) 0.0216(13) -0.1658(11) 0.060(3) Uani 1 1 d . . . . .
O2 O 0.7213(12) -0.0993(13) -0.2724(10) 0.058(3) Uani 1 1 d . . . . .
O3 O 0.7518(13) -0.2857(12) -0.0982(13) 0.066(3) Uani 1 1 d . . . . .
O4 O 0.5463(13) -0.2022(13) -0.0756(13) 0.067(3) Uani 1 1 d . . . . .
N1 N 0.7218(13) 0.0906(14) 0.1127(13) 0.051(3) Uani 1 1 d . U . . .
N2 N 0.8405(13) 0.0507(14) 0.0599(13) 0.044(3) Uani 1 1 d . . . . .
N3 N 0.9688(16) 0.1252(16) 0.1492(14) 0.062(4) Uani 1 1 d . . . . .
C1 C 0.6141(18) -0.0292(19) -0.2623(17) 0.051(4) Uani 1 1 d . . . . .
C2 C 0.5580(17) -0.0154(18) -0.3857(17) 0.053(4) Uani 1 1 d . . . . .
C3 C 0.614(2) -0.074(2) -0.5003(16) 0.076(6) Uani 1 1 d . . . . .
H3 H 0.691357 -0.122601 -0.502566 0.091 Uiso 1 1 calc R U . . .
C4 C 0.446(2) 0.060(2) -0.3870(18) 0.079(6) Uani 1 1 d . . . . .
H4 H 0.409471 0.102252 -0.308858 0.095 Uiso 1 1 calc R U . . .
C5 C 0.621(2) -0.2885(17) -0.0712(17) 0.054(4) Uani 1 1 d . . . . .
C6 C 0.5629(19) -0.3946(18) -0.0353(19) 0.060(5) Uani 1 1 d . . . . .
C7 C 0.427(2) -0.397(2) 0.006(2) 0.082(6) Uani 1 1 d . . . . .
H7 H 0.374019 -0.327338 0.008224 0.098 Uiso 1 1 calc R U . . .
C8 C 0.639(2) -0.500(2) -0.045(2) 0.079(7) Uani 1 1 d . . . . .
H8 H 0.729378 -0.505005 -0.075356 0.094 Uiso 1 1 calc R U . . .
C9A C 0.775(3) 0.225(3) 0.230(3) 0.033(7) Uani 0.5 1 d . U P A 1
H9A H 0.723532 0.291855 0.279037 0.040 Uiso 0.5 1 calc R U P A 1
C9B C 0.768(4) 0.167(4) 0.236(4) 0.045(9) Uani 0.5 1 d . U P A 2
H9B H 0.706649 0.208436 0.295056 0.054 Uiso 0.5 1 calc R U P A 2
C10A C 0.931(2) 0.222(3) 0.248(2) 0.032(5) Uani 0.6 1 d . U P A 1
H10A H 1.001454 0.286385 0.325744 0.039 Uiso 0.6 1 calc R U P A 1
C10B C 0.936319 0.184150 0.276419 0.084(19) Uani 0.4 1 d . U P A 2
H10B H 0.999620 0.222760 0.361521 0.101 Uiso 0.4 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'
Zn Zn 0.2839 1.4301 '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
N1 Zn1 N1 180.0 . 2_655
N1 Zn1 O1 91.7(5) . .
N1 Zn1 O1 88.3(5) 2_655 .
N1 Zn1 O1 88.3(5) . 2_655
N1 Zn1 O1 91.7(5) 2_655 2_655
O1 Zn1 O1 180.0 . 2_655
N1 Zn1 O4 91.6(5) . .
N1 Zn1 O4 88.4(5) 2_655 .
O1 Zn1 O4 90.6(5) . .
O1 Zn1 O4 89.4(5) 2_655 .
N1 Zn1 O4 88.4(5) . 2_655
N1 Zn1 O4 91.6(5) 2_655 2_655
O1 Zn1 O4 89.4(5) . 2_655
O1 Zn1 O4 90.6(5) 2_655 2_655
O4 Zn1 O4 180.0 . 2_655
O2 Zn2 O3 118.9(5) . .
O2 Zn2 N2 115.3(5) . .
O3 Zn2 N2 107.9(5) . .
O2 Zn2 N3 102.5(5) . 2_755
O3 Zn2 N3 104.3(6) . 2_755
N2 Zn2 N3 106.4(5) . 2_755
C1 O1 Zn1 144.6(11) . .
C1 O2 Zn2 120.2(10) . .
C5 O3 Zn2 110.4(10) . .
C5 O4 Zn1 152.6(13) . .
C9B N1 N2 108(2) . .
N2 N1 C9A 108.1(15) . .
C9B N1 Zn1 129.8(19) . .
N2 N1 Zn1 121.3(10) . .
C9A N1 Zn1 127.7(14) . .
N3 N2 N1 110.2(13) . .
N3 N2 Zn2 126.3(11) . .
N1 N2 Zn2 123.0(10) . .
C10A N3 N2 105.9(16) . .
N2 N3 C10B 108.4(12) . .
C10A N3 Zn2 126.4(14) . 2_755
N2 N3 Zn2 126.4(11) . 2_755
O1 C1 O2 126.6(14) . .
O1 C1 C2 119.3(16) . .
O2 C1 C2 114.2(15) . .
C3 C2 C4 117.7(15) . .
C3 C2 C1 122.4(15) . .
C4 C2 C1 119.9(16) . .
C2 C3 C4 119.4(15) . 2_654
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 2_654 .
C2 C4 C3 122.9(16) . 2_654
C2 C4 H4 118.5 . .
C3 C4 H4 118.5 2_654 .
O4 C5 O3 121.2(15) . .
O4 C5 C6 121.1(17) . .
O3 C5 C6 117.7(15) . .
C7 C6 C8 118.5(15) . .
C7 C6 C5 120.6(15) . .
C8 C6 C5 120.8(16) . .
C6 C7 C8 124.1(17) . 2_645
C6 C7 H7 118.0 . .
C8 C7 H7 118.0 2_645 .
C6 C8 C7 117.4(16) . 2_645
C6 C8 H8 121.3 . .
C7 C8 H8 121.3 2_645 .
C10A C9A N1 98(2) . .
C10A C9A H9A 131.1 . .
N1 C9A H9A 131.1 . .
N1 C9B C10B 111(3) . .
N1 C9B H9B 124.4 . .
C10B C9B H9B 124.4 . .
N3 C10A C9A 115(2) . .
N3 C10A H10A 122.4 . .
C9A C10A H10A 122.4 . .
N3 C10B C9B 98.8(16) . .
N3 C10B H10B 130.6 . .
C9B C10B H10B 130.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.088(12) .
Zn1 N1 2.088(12) 2_655
Zn1 O1 2.092(10) .
Zn1 O1 2.092(10) 2_655
Zn1 O4 2.092(12) .
Zn1 O4 2.092(12) 2_655
Zn2 O2 1.930(9) .
Zn2 O3 1.963(10) .
Zn2 N2 1.988(13) .
Zn2 N3 2.007(15) 2_755
O1 C1 1.204(19) .
O2 C1 1.298(19) .
O3 C5 1.268(19) .
O4 C5 1.233(18) .
N1 C9B 1.24(4) .
N1 N2 1.335(15) .
N1 C9A 1.44(3) .
N2 N3 1.326(16) .
N3 C10A 1.28(3) .
N3 C10B 1.383(14) .
C1 C2 1.484(19) .
C2 C3 1.37(2) .
C2 C4 1.38(2) .
C3 C4 1.39(2) 2_654
C3 H3 0.9300 .
C4 H4 0.9300 .
C5 C6 1.42(2) .
C6 C7 1.38(2) .
C6 C8 1.38(2) .
C7 C8 1.44(2) 2_645
C7 H7 0.9300 .
C8 H8 0.9300 .
C9A C10A 1.41(4) .
C9A H9A 0.9300 .
C9B C10B 1.50(4) .
C9B H9B 0.9300 .
C10A H10A 0.9300 .
C10B H10B 0.9300 .
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
_geom_torsion_site_symmetry_4
C9B N1 N2 N3 -11(2) . .
C9A N1 N2 N3 16(2) . .
Zn1 N1 N2 N3 178.5(9) . .
C9B N1 N2 Zn2 160.6(18) . .
C9A N1 N2 Zn2 -171.5(15) . .
Zn1 N1 N2 Zn2 -9.5(15) . .
N1 N2 N3 C10A -9(2) . .
Zn2 N2 N3 C10A 179.6(14) . .
N1 N2 N3 C10B 19.0(15) . .
Zn2 N2 N3 C10B -152.7(8) . .
N1 N2 N3 Zn2 -176.1(10) . 2_755
Zn2 N2 N3 Zn2 12.2(18) . 2_755
Zn1 O1 C1 O2 -31(3) . .
Zn1 O1 C1 C2 147.9(14) . .
Zn2 O2 C1 O1 -6(2) . .
Zn2 O2 C1 C2 175.0(10) . .
O1 C1 C2 C3 -178.1(18) . .
O2 C1 C2 C3 1(2) . .
O1 C1 C2 C4 2(3) . .
O2 C1 C2 C4 -178.6(16) . .
C4 C2 C3 C4 -2(3) . 2_654
C1 C2 C3 C4 178.5(17) . 2_654
C3 C2 C4 C3 2(3) . 2_654
C1 C2 C4 C3 -178.4(18) . 2_654
Zn1 O4 C5 O3 -73(3) . .
Zn1 O4 C5 C6 106(3) . .
Zn2 O3 C5 O4 8(2) . .
Zn2 O3 C5 C6 -171.5(13) . .
O4 C5 C6 C7 -5(3) . .
O3 C5 C6 C7 174.8(18) . .
O4 C5 C6 C8 172.8(19) . .
O3 C5 C6 C8 -7(3) . .
C8 C6 C7 C8 3(4) . 2_645
C5 C6 C7 C8 -179.4(18) . 2_645
C7 C6 C8 C7 -2(3) . 2_645
C5 C6 C8 C7 179.6(17) . 2_645
N2 N1 C9A C10A -16(3) . .
Zn1 N1 C9A C10A -176.6(14) . .
N2 N1 C9B C10B 0(3) . .
Zn1 N1 C9B C10B 168.8(10) . .
N2 N3 C10A C9A -3(3) . .
Zn2 N3 C10A C9A 164.6(18) 2_755 .
N1 C9A C10A N3 12(3) . .
N2 N3 C10B C9B -17.0(17) . .
Zn2 N3 C10B C9B 177.5(16) 2_755 .
N1 C9B C10B N3 11(3) . .
