#------------------------------------------------------------------------------
#$Date: 2017-12-26 01:38:15 +0200 (Tue, 26 Dec 2017) $
#$Revision: 204517 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/69/4126907.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_4126907
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_moiety         'C20 H12 N6 O8 Zn3'
_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_date             2017-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_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       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_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  0.1075
_diffrn_reflns_av_unetI/netI     0.1754
_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            6746
_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          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0890
_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)+(0.0852P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1726
_reflns_number_total             3375
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            1eII_squeeze.cif
_cod_data_source_block           1eII_squeeze
_cod_database_code               4126907
_shelx_shelxl_version_number     2017/1
_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_max   0.863
_shelx_estimated_absorpt_t_min   0.680
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9A) \\sim Ueq, Uanis(C9B) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.01
Uanis(C10B) \\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.01
3. Others
 Fixed Sof: C9A(0.5) H9A(0.5) C9B(0.5) H9B(0.5) C10A(0.6) H10A(0.6) C10B(0.4)
 H10B(0.4)
 Fixed X: C10B(0.936319)
 Fixed Y: C10B(0.18415)
 Fixed Z: C10B(0.276419)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9A(H9A), C9B(H9B), C10A(H10A), C10B(H10B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
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 0.0463(5) Uani 1 2 d S T P A .
Zn2 Zn 0.81991(11) -0.11577(13) -0.11813(12) 0.0438(4) Uani 1 1 d . . . . .
O1 O 0.5576(8) 0.0197(8) -0.1661(7) 0.062(2) Uani 1 1 d . . . . .
O2 O 0.7225(7) -0.0999(8) -0.2706(6) 0.058(2) Uani 1 1 d . . . . .
O3 O 0.7520(8) -0.2840(7) -0.0988(7) 0.062(2) Uani 1 1 d . . . . .
O4 O 0.5448(8) -0.2003(7) -0.0757(8) 0.066(2) Uani 1 1 d . . . . .
N1 N 0.7213(8) 0.0908(9) 0.1128(8) 0.052(2) Uani 1 1 d . U . . .
N2 N 0.8414(9) 0.0527(8) 0.0621(8) 0.0411(19) Uani 1 1 d . . . . .
N3 N 0.9720(10) 0.1277(9) 0.1500(8) 0.059(2) Uani 1 1 d . . . . .
C1 C 0.6147(11) -0.0324(11) -0.2647(10) 0.046(3) Uani 1 1 d . . . . .
C2 C 0.5581(10) -0.0190(10) -0.3863(10) 0.045(3) Uani 1 1 d . . . . .
C3 C 0.6106(12) -0.0765(12) -0.5020(9) 0.062(3) Uani 1 1 d . . . . .
H3 H 0.684365 -0.129643 -0.506959 0.075 Uiso 1 1 calc R . . . .
C4 C 0.4436(13) 0.0571(13) -0.3890(11) 0.079(4) Uani 1 1 d . . . . .
H4 H 0.403078 0.096064 -0.312493 0.094 Uiso 1 1 calc R . . . .
C5 C 0.6172(12) -0.2895(11) -0.0721(11) 0.054(3) Uani 1 1 d . . . . .
C6 C 0.5594(11) -0.3951(10) -0.0346(11) 0.054(3) Uani 1 1 d . . . . .
C7 C 0.4269(13) -0.3976(13) 0.0075(12) 0.076(4) Uani 1 1 d . . . . .
H7 H 0.374346 -0.327290 0.013393 0.091 Uiso 1 1 calc R . . . .
C8 C 0.6335(13) -0.5017(12) -0.0417(12) 0.079(4) Uani 1 1 d . . . . .
H8 H 0.725099 -0.504958 -0.069916 0.094 Uiso 1 1 calc R . . . .
C9A C 0.7766(17) 0.2241(19) 0.2241(17) 0.024(4) Uani 0.5 1 d . U . A 1
H9A H 0.725393 0.292277 0.272173 0.029 Uiso 0.5 1 calc R . . A 1
C9B C 0.773(2) 0.170(2) 0.2426(19) 0.032(5) Uani 0.5 1 d . U . A 2
H9B H 0.714026 0.210490 0.304386 0.039 Uiso 0.5 1 calc R . . A 2
C10A C 0.9332(14) 0.2239(15) 0.2413(14) 0.024(3) Uani 0.6 1 d . U . A 1
H10A H 1.003233 0.292417 0.317100 0.029 Uiso 0.6 1 calc R . . A 1
C10B C 0.936319 0.184150 0.276419 0.060(9) Uani 0.4 1 d . U . A 2
H10B H 1.000341 0.221647 0.361073 0.072 Uiso 0.4 1 calc R . . 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
O1 Zn1 O1 180.00(10) . 2_655
O4 Zn1 O1 90.0(3) 2_655 2_655
O4 Zn1 O1 90.0(3) . .
O4 Zn1 O1 90.0(3) . 2_655
O4 Zn1 O1 90.0(3) 2_655 .
O4 Zn1 O4 180.0 . 2_655
O4 Zn1 N1 92.0(3) 2_655 2_655
O4 Zn1 N1 88.0(3) . 2_655
O4 Zn1 N1 92.0(3) . .
O4 Zn1 N1 88.0(3) 2_655 .
N1 Zn1 O1 88.1(3) . 2_655
N1 Zn1 O1 88.1(3) 2_655 .
N1 Zn1 O1 91.9(3) 2_655 2_655
N1 Zn1 O1 91.9(3) . .
N1 Zn1 N1 180.0 . 2_655
O2 Zn2 O3 118.8(3) . .
O2 Zn2 N2 115.5(3) . .
O2 Zn2 N3 102.6(3) . 2_755
O3 Zn2 N2 107.9(3) . .
O3 Zn2 N3 103.8(3) . 2_755
N3 Zn2 N2 106.7(3) 2_755 .
C1 O1 Zn1 145.0(7) . .
C1 O2 Zn2 122.0(6) . .
C5 O3 Zn2 111.5(6) . .
C5 O4 Zn1 153.3(8) . .
N2 N1 Zn1 122.2(6) . .
N2 N1 C9A 105.6(9) . .
C9A N1 Zn1 128.5(8) . .
C9B N1 Zn1 131.0(10) . .
C9B N1 N2 105.7(10) . .
N1 N2 Zn2 121.8(6) . .
N1 N2 N3 112.2(8) . .
N3 N2 Zn2 125.6(6) . .
N2 N3 Zn2 127.0(6) . 2_755
N2 N3 C10B 106.1(7) . .
C10A N3 Zn2 127.5(9) . 2_755
C10A N3 N2 103.7(10) . .
O1 C1 O2 124.8(8) . .
O1 C1 C2 119.0(10) . .
O2 C1 C2 116.2(9) . .
C3 C2 C1 123.5(10) . .
C3 C2 C4 115.7(9) . .
C4 C2 C1 120.7(10) . .
C2 C3 H3 119.6 . .
C2 C3 C4 120.9(9) . 2_654
C4 C3 H3 119.6 2_654 .
C2 C4 H4 118.3 . .
C3 C4 C2 123.4(10) 2_654 .
C3 C4 H4 118.3 2_654 .
O3 C5 C6 118.7(9) . .
O4 C5 O3 119.1(9) . .
O4 C5 C6 122.2(10) . .
C7 C6 C5 121.5(9) . .
C7 C6 C8 116.2(9) . .
C8 C6 C5 122.2(10) . .
C6 C7 H7 118.4 . .
C6 C7 C8 123.3(10) . 2_645
C8 C7 H7 118.4 2_645 .
C6 C8 H8 119.8 . .
C7 C8 C6 120.5(10) 2_645 .
C7 C8 H8 119.8 2_645 .
N1 C9A H9A 130.4 . .
N1 C9A C10A 99.2(13) . .
C10A C9A H9A 130.4 . .
N1 C9B H9B 124.8 . .
N1 C9B C10B 110.3(14) . .
C10B C9B H9B 124.8 . .
N3 C10A C9A 116.3(14) . .
N3 C10A H10A 121.9 . .
C9A C10A H10A 121.9 . .
N3 C10B C9B 102.1(8) . .
N3 C10B H10B 129.0 . .
C9B C10B H10B 129.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.086(6) 2_655
Zn1 O1 2.086(6) .
Zn1 O4 2.068(7) 2_655
Zn1 O4 2.068(7) .
Zn1 N1 2.085(7) .
Zn1 N1 2.085(7) 2_655
Zn2 O2 1.902(6) .
Zn2 O3 1.941(6) .
Zn2 N2 2.016(8) .
Zn2 N3 1.985(9) 2_755
O1 C1 1.228(11) .
O2 C1 1.288(11) .
O3 C5 1.301(11) .
O4 C5 1.244(11) .
N1 N2 1.331(9) .
N1 C9A 1.404(18) .
N1 C9B 1.309(19) .
N2 N3 1.336(9) .
N3 C10A 1.236(14) .
N3 C10B 1.386(8) .
C1 C2 1.464(11) .
C2 C3 1.361(12) .
C2 C4 1.412(13) .
C3 H3 0.9300 .
C3 C4 1.365(12) 2_654
C4 H4 0.9300 .
C5 C6 1.431(12) .
C6 C7 1.353(13) .
C6 C8 1.383(13) .
C7 H7 0.9300 .
C7 C8 1.369(12) 2_645
C8 H8 0.9300 .
C9A H9A 0.9300 .
C9A C10A 1.413(19) .
C9B H9B 0.9300 .
C9B C10B 1.453(18) .
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
Zn1 O1 C1 O2 -32.0(18) . .
Zn1 O1 C1 C2 147.7(8) . .
Zn1 O4 C5 O3 -74(2) . .
Zn1 O4 C5 C6 103.6(16) . .
Zn1 N1 N2 Zn2 -9.4(9) . .
Zn1 N1 N2 N3 177.8(6) . .
Zn1 N1 C9A C10A -174.0(8) . .
Zn1 N1 C9B C10B 168.7(6) . .
Zn2 O2 C1 O1 -4.9(14) . .
Zn2 O2 C1 C2 175.3(6) . .
Zn2 O3 C5 O4 7.1(13) . .
Zn2 O3 C5 C6 -170.6(8) . .
Zn2 N2 N3 Zn2 10.5(11) . 2_755
Zn2 N2 N3 C10A 176.4(8) . .
Zn2 N2 N3 C10B -152.6(4) . .
Zn2 N3 C10A C9A 165.4(10) 2_755 .
Zn2 N3 C10B C9B 178.9(9) 2_755 .
O1 C1 C2 C3 -178.0(10) . .
O1 C1 C2 C4 2.4(15) . .
O2 C1 C2 C3 1.8(15) . .
O2 C1 C2 C4 -177.8(9) . .
O3 C5 C6 C7 173.3(11) . .
O3 C5 C6 C8 -8.0(17) . .
O4 C5 C6 C7 -4.4(18) . .
O4 C5 C6 C8 174.3(11) . .
N1 N2 N3 Zn2 -176.9(6) . 2_755
N1 N2 N3 C10A -11.0(12) . .
N1 N2 N3 C10B 20.0(9) . .
N1 C9A C10A N3 10.5(17) . .
N1 C9B C10B N3 10.6(14) . .
N2 N1 C9A C10A -15.7(13) . .
N2 N1 C9B C10B 0.8(15) . .
N2 N3 C10A C9A -0.4(16) . .
N2 N3 C10B C9B -17.5(10) . .
C1 C2 C3 C4 -178.1(10) . 2_654
C1 C2 C4 C3 178.1(10) . 2_654
C3 C2 C4 C3 -1.5(19) . 2_654
C4 C2 C3 C4 1.5(19) . 2_654
C5 C6 C7 C8 178.7(11) . 2_645
C5 C6 C8 C7 -178.7(11) . 2_645
C7 C6 C8 C7 0(2) . 2_645
C8 C6 C7 C8 0(2) . 2_645
C9A N1 N2 Zn2 -169.4(8) . .
C9A N1 N2 N3 17.8(12) . .
C9B N1 N2 Zn2 159.9(9) . .
C9B N1 N2 N3 -12.9(13) . .
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 -0.015 -0.036 0.474 473 101 ' '
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.593 -0.128 -0.160 490.8 114.6
