 
data_b-ZIF-65(Zn)

# start Validation Reply Form
_vrf_PLAT919_b-ZIF-65Zn
;
PROBLEM: Reflection # Likely Affected by the Beamstop ... 2 Check
RESPONSE: The reflections (2 3 3), (1 1 2), and (1 1 4) had
large D = (Fo**2 - Fc**2) / sqrt(weight) values greater 10 with low 
resolutions (< 8 A).
Thus, these reflections were not included for the final 
refinement using the OMIT instruction.
However, the other four reflections (2 8 8), (2 2 10),
(6 4 8), and (4 6 8) having large D values (10.20~10.71)
were not omitted due to relatively higher 
resolutions (3.00~3.32 A).
;
# end Validation Reply Form

_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             'b-ZIF-65(Zn)'
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C12 H8 N12 O8 Zn2 [+ solvent]'
_chemical_formula_sum
 'C12 H8 N12 O8 Zn2' 
_chemical_formula_weight          579.04

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0020   0.0010
 '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'   0.0040   0.0020
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0080   0.0040
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn'  'Zn'   0.3510   1.1150
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            206
_space_group_name_H-M_alt         'I a -3'
_space_group_name_Hall            '-I 2b 2c 3'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 'z, x, y'
 'z+1/2, -x+1/2, -y'
 '-z+1/2, -x, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y, z, x'
 '-y, z+1/2, -x+1/2'
 'y+1/2, -z+1/2, -x'
 '-y+1/2, -z, x+1/2'
 'x+1/2, y+1/2, z+1/2'
 '-x+1, -y+1/2, z+1'
 '-x+1/2, y+1, -z+1'
 'x+1, -y+1, -z+1/2'
 'z+1/2, x+1/2, y+1/2'
 'z+1, -x+1, -y+1/2'
 '-z+1, -x+1/2, y+1'
 '-z+1/2, x+1, -y+1'
 'y+1/2, z+1/2, x+1/2'
 '-y+1/2, z+1, -x+1'
 'y+1, -z+1, -x+1/2'
 '-y+1, -z+1/2, x+1'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 '-z, -x, -y'
 '-z-1/2, x-1/2, y'
 'z-1/2, x, -y-1/2'
 'z, -x-1/2, y-1/2'
 '-y, -z, -x'
 'y, -z-1/2, x-1/2'
 '-y-1/2, z-1/2, x'
 'y-1/2, z, -x-1/2'
 '-x+1/2, -y+1/2, -z+1/2'
 'x, y+1/2, -z'
 'x+1/2, -y, z'
 '-x, y, z+1/2'
 '-z+1/2, -x+1/2, -y+1/2'
 '-z, x, y+1/2'
 'z, x+1/2, -y'
 'z+1/2, -x, y'
 '-y+1/2, -z+1/2, -x+1/2'
 'y+1/2, -z, x'
 '-y, z, x+1/2'
 'y, z+1/2, -x'
 
_cell_length_a                    34.502(4)
_cell_length_b                    34.502(4)
_cell_length_c                    34.502(4)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      41071(14)
_cell_formula_units_Z             48
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     184479
_cell_measurement_theta_min       0.716
_cell_measurement_theta_max       23.994
 
_exptl_crystal_description        block
_exptl_crystal_colour             'dark yellow'
_exptl_crystal_density_meas       none
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.124          
_exptl_crystal_F_000              13824
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.230
_exptl_crystal_size_mid           0.220
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     0.955
_shelx_estimated_absorpt_T_min    0.810
_shelx_estimated_absorpt_T_max    0.911
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.610
_diffrn_radiation_type            synchrotron
_diffrn_source                    'PLSII 2D bending magnet'
_diffrn_measurement_device_type   'ADSC Q210 CCD area detector'
_diffrn_measurement_method        'omega scan'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             16640
_diffrn_reflns_av_unetI/netI      0.0417
_diffrn_reflns_av_R_equivalents   0.0239
_diffrn_reflns_limit_h_min        -45
_diffrn_reflns_limit_h_max        46
_diffrn_reflns_limit_k_min        -32
_diffrn_reflns_limit_k_max        32
_diffrn_reflns_limit_l_min        -31
_diffrn_reflns_limit_l_max        31
_diffrn_reflns_theta_min          0.716
_diffrn_reflns_theta_max          23.994
_diffrn_reflns_theta_full         21.469
_diffrn_measured_fraction_theta_max   0.989
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.989
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.989
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              8412
_reflns_number_gt                 5989
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
 
_computing_data_collection        'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement        'HKL3000'
_computing_data_reduction         'HKL3000'
_computing_structure_solution     'SHELX-S'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     'Bruker SHELX-TL XP'
_computing_publication_material   'SHELX ciftab'
_refine_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0923P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.000065(15)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          8412
_refine_ls_number_parameters      310
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0680
_refine_ls_R_factor_gt            0.0467
_refine_ls_wR_factor_ref          0.1499
_refine_ls_wR_factor_gt           0.1433
_refine_ls_goodness_of_fit_ref    1.069
_refine_ls_restrained_S_all       1.069
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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 0.000000 0.750000 0.11702(2) 0.03703(19) Uani 1 2 d S T P . .
Zn2 Zn 0.000000 0.750000 -0.13282(2) 0.03232(18) Uani 1 2 d S T P . .
Zn3 Zn 0.12508(2) 0.75846(2) -0.00760(2) 0.03607(13) Uani 1 1 d . . . . .
C1 C 0.08510(13) 0.72775(14) 0.10221(14) 0.0468(11) Uani 1 1 d . . . . .
H1 H 0.087231 0.713331 0.125568 0.056 Uiso 1 1 calc R U . . .
C2 C 0.11226(13) 0.73044(13) 0.07504(13) 0.0443(10) Uani 1 1 d . . . . .
H2 H 0.137187 0.718814 0.076269 0.053 Uiso 1 1 calc R U . . .
C3 C 0.06381(12) 0.76209(12) 0.05685(13) 0.0361(10) Uani 1 1 d . . . . .
C4 C 0.10574(13) 0.78813(15) -0.08888(14) 0.0523(12) Uani 1 1 d . . . . .
H4 H 0.127579 0.804893 -0.089106 0.063 Uiso 1 1 calc R U . . .
C5 C 0.07892(14) 0.78591(13) -0.11712(13) 0.0472(12) Uani 1 1 d . . . . .
H5 H 0.078848 0.800067 -0.140737 0.057 Uiso 1 1 calc R U . . .
C6 C 0.06376(12) 0.74770(12) -0.06990(12) 0.0320(9) Uani 1 1 d . . . . .
C7 C 0.14290(14) 0.67929(14) -0.03916(16) 0.0581(14) Uani 1 1 d . . . . .
H7 H 0.120421 0.678790 -0.055054 0.070 Uiso 1 1 calc R U . . .
C8 C 0.17264(14) 0.65067(16) -0.03763(15) 0.0577(14) Uani 1 1 d . . . . .
H8 H 0.174070 0.628408 -0.053762 0.069 Uiso 1 1 calc R U . . .
C9 C 0.18602(13) 0.69505(13) 0.00217(14) 0.0393(10) Uani 1 1 d . . . . .
C10 C 0.02151(16) 0.66509(14) 0.12986(16) 0.0624(15) Uani 1 1 d . . . . .
H10 H 0.036090 0.662962 0.106599 0.075 Uiso 1 1 calc R U . . .
C11 C 0.01701(15) 0.63533(15) 0.15925(14) 0.0581(14) Uani 1 1 d . . . . .
H11 H 0.027122 0.609749 0.157989 0.070 Uiso 1 1 calc R U . . .
C12 C -0.01328(13) 0.68547(13) 0.17598(13) 0.0419(11) Uani 1 1 d . . . . .
N1 N 0.05299(11) 0.74952(11) 0.09092(11) 0.0379(9) Uani 1 1 d . . . . .
N2 N 0.09871(11) 0.75262(11) 0.04492(12) 0.0404(9) Uani 1 1 d . . . . .
N3 N 0.04010(11) 0.78779(10) 0.03501(11) 0.0437(8) Uani 1 1 d . . . . .
N4 N 0.09658(10) 0.76181(11) -0.05882(11) 0.0381(9) Uani 1 1 d . . . . .
N5 N 0.05099(11) 0.75871(11) -0.10512(11) 0.0402(9) Uani 1 1 d . . . . .
N6 N 0.04421(11) 0.71917(10) -0.04935(11) 0.0426(9) Uani 1 1 d . . . . .
N7 N 0.15288(11) 0.70730(12) -0.01363(11) 0.0447(10) Uani 1 1 d . . . . .
N8 N 0.19885(11) 0.66014(12) -0.00935(11) 0.0418(9) Uani 1 1 d . . . . .
N9 N 0.20757(10) 0.71732(10) 0.03043(10) 0.0410(8) Uani 1 1 d . . . . .
N10 N 0.00087(11) 0.69678(12) 0.14182(12) 0.0460(10) Uani 1 1 d . . . . .
N11 N -0.00363(12) 0.64996(11) 0.18816(13) 0.0465(11) Uani 1 1 d . . . . .
N12 N -0.03933(11) 0.71052(11) 0.19864(10) 0.0440(9) Uani 1 1 d . . . . .
O1 O 0.00663(10) 0.79457(10) 0.04832(10) 0.0552(9) Uani 1 1 d . . . . .
O2 O 0.05245(10) 0.80083(10) 0.00426(10) 0.0503(8) Uani 1 1 d . . . . .
O3 O 0.05756(10) 0.71023(10) -0.01697(10) 0.0551(9) Uani 1 1 d . . . . .
O4 O 0.01419(11) 0.70477(10) -0.06335(10) 0.0584(10) Uani 1 1 d . . . . .
O5 O 0.19410(9) 0.75006(10) 0.03883(10) 0.0488(9) Uani 1 1 d . . . . .
O6 O 0.23666(10) 0.70308(9) 0.04514(10) 0.0496(8) Uani 1 1 d . . . . .
O7 O -0.04654(10) 0.74286(10) 0.18528(10) 0.0497(9) Uani 1 1 d . . . . .
O8 O -0.05261(10) 0.69761(10) 0.22831(9) 0.0524(8) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Zn1 N10 2.026(4) . ?
Zn1 N10 2.026(4) 14_464 ?
Zn1 N1 2.038(4) . ?
Zn1 N1 2.038(4) 14_464 ?
Zn2 N8 2.026(4) 8 ?
Zn2 N8 2.026(4) 18_455 ?
Zn2 N5 2.025(4) 14_464 ?
Zn2 N5 2.025(4) . ?
Zn3 N7 2.020(4) . ?
Zn3 N4 2.026(4) . ?
Zn3 N2 2.038(4) . ?
Zn3 N11 2.036(4) 46_465 ?
C1 C2 1.329(6) . ?
C1 N1 1.394(6) . ?
C2 N2 1.373(6) . ?
C3 N1 1.307(6) . ?
C3 N2 1.314(6) . ?
C3 N3 1.423(5) . ?
C4 C5 1.346(6) . ?
C4 N4 1.414(6) . ?
C5 N5 1.407(5) . ?
C6 N4 1.290(6) . ?
C6 N5 1.347(6) . ?
C6 N6 1.388(5) . ?
C7 N7 1.352(6) . ?
C7 C8 1.425(7) . ?
C8 N8 1.370(6) . ?
C9 N7 1.335(6) . ?
C9 N8 1.344(6) . ?
C9 N9 1.447(5) . ?
C10 N10 1.368(6) . ?
C10 C11 1.452(7) . ?
C11 N11 1.325(6) . ?
C12 N10 1.334(6) . ?
C12 N11 1.337(6) . ?
C12 N12 1.472(6) . ?
N3 O2 1.229(5) . ?
N3 O1 1.264(5) . ?
N6 O4 1.246(5) . ?
N6 O3 1.247(5) . ?
N9 O6 1.227(4) . ?
N9 O5 1.255(5) . ?
N12 O8 1.207(4) . ?
N12 O7 1.233(5) . ?
 
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
 _geom_angle_publ_flag
N10 Zn1 N10 130.0(2) . 14_464 ?
N10 Zn1 N1 99.55(14) . . ?
N10 Zn1 N1 101.97(14) 14_464 . ?
N10 Zn1 N1 101.97(14) . 14_464 ?
N10 Zn1 N1 99.55(14) 14_464 14_464 ?
N1 Zn1 N1 127.6(2) . 14_464 ?
N8 Zn2 N8 124.6(2) 8 18_455 ?
N8 Zn2 N5 103.21(17) 8 14_464 ?
N8 Zn2 N5 102.15(16) 18_455 14_464 ?
N8 Zn2 N5 102.16(16) 8 . ?
N8 Zn2 N5 103.21(17) 18_455 . ?
N5 Zn2 N5 123.7(2) 14_464 . ?
N7 Zn3 N4 100.98(16) . . ?
N7 Zn3 N2 102.54(15) . . ?
N4 Zn3 N2 124.38(16) . . ?
N7 Zn3 N11 126.67(17) . 46_465 ?
N4 Zn3 N11 102.22(15) . 46_465 ?
N2 Zn3 N11 102.59(17) . 46_465 ?
C2 C1 N1 109.0(4) . . ?
C1 C2 N2 109.4(4) . . ?
N1 C3 N2 117.4(4) . . ?
N1 C3 N3 121.3(4) . . ?
N2 C3 N3 121.1(4) . . ?
C5 C4 N4 109.9(4) . . ?
C4 C5 N5 107.2(4) . . ?
N4 C6 N5 116.6(4) . . ?
N4 C6 N6 122.9(4) . . ?
N5 C6 N6 120.1(4) . . ?
N7 C7 C8 106.7(4) . . ?
N8 C8 C7 109.7(4) . . ?
N7 C9 N8 116.4(4) . . ?
N7 C9 N9 123.2(4) . . ?
N8 C9 N9 120.4(4) . . ?
N10 C10 C11 107.4(5) . . ?
N11 C11 C10 108.3(4) . . ?
N10 C12 N11 117.0(4) . . ?
N10 C12 N12 121.4(4) . . ?
N11 C12 N12 121.5(4) . . ?
C3 N1 C1 101.7(4) . . ?
C3 N1 Zn1 130.6(3) . . ?
C1 N1 Zn1 126.4(3) . . ?
C3 N2 C2 102.3(4) . . ?
C3 N2 Zn3 131.6(3) . . ?
C2 N2 Zn3 125.2(3) . . ?
O2 N3 O1 124.3(4) . . ?
O2 N3 C3 119.1(4) . . ?
O1 N3 C3 116.6(4) . . ?
C6 N4 C4 102.8(4) . . ?
C6 N4 Zn3 131.5(3) . . ?
C4 N4 Zn3 124.6(3) . . ?
C6 N5 C5 103.3(4) . . ?
C6 N5 Zn2 131.9(3) . . ?
C5 N5 Zn2 123.7(3) . . ?
O4 N6 O3 123.7(4) . . ?
O4 N6 C6 119.2(4) . . ?
O3 N6 C6 117.0(4) . . ?
C9 N7 C7 104.9(4) . . ?
C9 N7 Zn3 129.9(3) . . ?
C7 N7 Zn3 124.8(3) . . ?
C9 N8 C8 101.9(4) . . ?
C9 N8 Zn2 131.1(3) . 11_455 ?
C8 N8 Zn2 125.3(3) . 11_455 ?
O6 N9 O5 124.6(4) . . ?
O6 N9 C9 119.1(4) . . ?
O5 N9 C9 116.3(4) . . ?
C12 N10 C10 102.9(4) . . ?
C12 N10 Zn1 129.3(3) . . ?
C10 N10 Zn1 127.2(3) . . ?
C11 N11 C12 104.2(4) . . ?
C11 N11 Zn3 123.8(3) . 43_556 ?
C12 N11 Zn3 130.8(3) . 43_556 ?
O8 N12 O7 125.1(4) . . ?
O8 N12 C12 117.7(4) . . ?
O7 N12 C12 117.1(4) . . ?
 
_refine_diff_density_max    0.761
_refine_diff_density_min   -0.538
_refine_diff_density_rms    0.084




