#------------------------------------------------------------------------------
#$Date: 2021-11-06 22:10:47 +0200 (Sat, 06 Nov 2021) $
#$Revision: 270454 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/24/1562409.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_1562409
loop_
_publ_author_name
'Ge, Meng'
'Yang, Taimin'
'Wang, Yanzhi'
'Carraro, Francesco'
'Liang, Weibin'
'Doonan, Christian'
'Falcaro, Paolo'
'Zheng, Haoquan'
'Zou, Xiaodong'
'Huang, Zhehao'
_publ_section_title
;
 On the completeness of three-dimensional electron diffraction data for
 structural analysis of metal-organic frameworks.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              66
_journal_page_last               80
_journal_paper_doi               10.1039/d1fd00020a
_journal_volume                  231
_journal_year                    2021
_chemical_formula_sum            'C10 N5 O0.5 Zn1.5'
_chemical_formula_weight         296.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-19 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.162(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6540(19)
_cell_length_b                   14.936(3)
_cell_length_c                   14.311(2)
_cell_measurement_reflns_used    5093
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.899
_cell_measurement_theta_min      0.014
_cell_volume                     2573.0(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'JEOL JEM-2100 LaB6'
_diffrn_measurement_method       'Continuous rotation electron diffraction'
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.1679
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43219
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.922
_diffrn_reflns_theta_min         0.075
_diffrn_source                   'electron microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       nano-crystals
_exptl_crystal_F_000             370
_exptl_crystal_size_max          0.0005
_exptl_crystal_size_mid          0.0005
_exptl_crystal_size_min          0.0003
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       1169(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.719
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5093
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.675
_refine_ls_R_factor_all          0.1927
_refine_ls_R_factor_gt           0.1726
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4634
_refine_ls_wR_factor_ref         0.4749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3933
_reflns_number_total             5093
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1fd00020a1.cif
_cod_data_source_block           M_ABC
_cod_depositor_comments
'Adding full bibliography for 1562402--1562412.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C10 N5 O0.50 Zn1.50'
_cod_database_code               1562409
_shelx_shelxl_version_number     2018/3
_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Zn1 Zn 0.2839(2) 0.37181(14) 0.75935(18) 0.0509(7) Uani 1 1 d . . . . .
Zn2 Zn 0.1233(3) 0.64765(17) 0.9761(2) 0.0597(8) Uani 1 1 d . . . . .
Zn3 Zn 0.3005(3) 0.65727(17) 0.4573(2) 0.0581(8) Uani 1 1 d . . . . .
N1 N 0.1973(8) 0.6133(5) 0.1329(6) 0.065(2) Uani 1 1 d D . . . .
N2 N 0.2558(8) 0.6152(4) 0.3078(6) 0.065(2) Uani 1 1 d D . . . .
N3 N 0.3347(8) 0.5506(5) 0.5579(6) 0.071(2) Uani 1 1 d D . . . .
N4 N 0.3368(8) 0.4546(5) 0.6786(6) 0.0632(19) Uani 1 1 d D . . . .
N5 N 0.4088(7) 0.3118(5) 0.8886(5) 0.0578(18) Uani 1 1 d D . . . .
N6 N 0.5555(8) 0.2273(5) 0.9871(5) 0.065(2) Uani 1 1 d D . . . .
N7 N 0.1853(8) 0.2764(5) 0.6573(6) 0.063(2) Uani 1 1 d D . . . .
N8 N 0.0401(8) 0.1820(5) 0.5741(5) 0.065(2) Uani 1 1 d D . . . .
N9 N 0.1895(7) 0.4448(4) 0.8069(6) 0.0584(17) Uani 1 1 d D . . . .
N10 N 0.1317(8) 0.5465(5) 0.8882(6) 0.0640(19) Uani 1 1 d D . . . .
O1 O 0.1789(9) 0.7339(5) 0.4536(7) 0.076(2) Uani 1 1 d . . . . .
C1 C 0.1095(8) 0.2220(5) 0.6673(6) 0.061(2) Uani 1 1 d D . . . .
C2 C 0.2732(8) 0.5047(5) 0.5911(6) 0.061(2) Uani 1 1 d D . . . .
C3 C 0.2181(7) 0.5098(4) 0.8803(6) 0.0567(19) Uani 1 1 d D . . . .
C4 C 0.2156(7) 0.6652(5) 0.2169(6) 0.061(2) Uani 1 1 d D . . . .
C5 C 0.4930(8) 0.2650(6) 0.8906(6) 0.084(3) Uani 1 1 d D . . . .
C6 C 0.1488(9) 0.5086(7) 0.5382(8) 0.087(3) Uani 1 1 d D . . . .
C7 C 0.3358(10) 0.5405(7) 0.9468(9) 0.091(3) Uani 1 1 d D . . . .
C8 C 0.5029(9) 0.2501(6) 1.0457(6) 0.072(3) Uani 1 1 d D . . . .
C9 C 0.4107(10) 0.3024(6) 0.9835(7) 0.073(3) Uani 1 1 d D . . . .
C10 C 0.2619(9) 0.5268(5) 0.2786(6) 0.066(3) Uani 1 1 d D . . . .
C11 C 0.0785(10) 0.2044(6) 0.5040(7) 0.076(3) Uani 1 1 d D . . . .
C12 C 0.0746(8) 0.4386(6) 0.7618(7) 0.066(2) Uani 1 1 d D . . . .
C13 C 0.1665(10) 0.2628(6) 0.5549(7) 0.074(3) Uani 1 1 d D . . . .
C14 C 0.0404(9) 0.5003(6) 0.8140(7) 0.072(2) Uani 1 1 d D . . . .
C15 C 0.1036(11) 0.2118(6) 0.7688(7) 0.083(4) Uani 1 1 d D . . . .
C16 C 0.2241(10) 0.5265(6) 0.1680(6) 0.076(3) Uani 1 1 d D . . . .
C17 C 0.4454(10) 0.4701(6) 0.7033(9) 0.081(3) Uani 1 1 d D . . . .
C18 C 0.4434(10) 0.5287(8) 0.6276(9) 0.091(3) Uani 1 1 d D . . . .
C19 C 0.1972(11) 0.7649(5) 0.2132(8) 0.080(3) Uani 1 1 d D . . . .
C20 C 0.5189(11) 0.2530(7) 0.8009(7) 0.084(3) Uani 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 '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
_geom_angle_publ_flag
N7 Zn1 N9 107.9(4) . . ?
N7 Zn1 N4 108.1(3) . . ?
N9 Zn1 N4 108.3(3) . . ?
N7 Zn1 N5 109.3(3) . . ?
N9 Zn1 N5 108.8(3) . . ?
N4 Zn1 N5 114.3(4) . . ?
N10 Zn2 O1 115.1(3) . 4_576 ?
N10 Zn2 N1 110.8(3) . 1_556 ?
O1 Zn2 N1 111.6(4) 4_576 1_556 ?
N10 Zn2 N8 110.0(4) . 2_556 ?
O1 Zn2 N8 98.9(4) 4_576 2_556 ?
N1 Zn2 N8 109.8(3) 1_556 2_556 ?
O1 Zn3 N2 108.6(4) . . ?
O1 Zn3 N6 110.8(4) . 2_656 ?
N2 Zn3 N6 109.1(3) . 2_656 ?
O1 Zn3 N3 112.0(4) . . ?
N2 Zn3 N3 110.8(3) . . ?
N6 Zn3 N3 105.5(4) 2_656 . ?
C4 N1 C16 108.1(7) . . ?
C4 N1 Zn2 128.4(6) . 1_554 ?
C16 N1 Zn2 123.1(5) . 1_554 ?
C4 N2 C10 106.5(6) . . ?
C4 N2 Zn3 128.2(5) . . ?
C10 N2 Zn3 125.3(5) . . ?
C2 N3 C18 105.3(8) . . ?
C2 N3 Zn3 132.7(7) . . ?
C18 N3 Zn3 120.2(7) . . ?
C2 N4 C17 106.6(7) . . ?
C2 N4 Zn1 127.6(7) . . ?
C17 N4 Zn1 125.7(6) . . ?
C5 N5 C9 108.4(7) . . ?
C5 N5 Zn1 126.4(5) . . ?
C9 N5 Zn1 124.6(6) . . ?
C5 N6 C8 105.0(7) . . ?
C5 N6 Zn3 129.9(6) . 2_646 ?
C8 N6 Zn3 125.1(6) . 2_646 ?
C13 N7 C1 104.6(7) . . ?
C13 N7 Zn1 126.6(6) . . ?
C1 N7 Zn1 128.0(5) . . ?
C1 N8 C11 106.2(8) . . ?
C1 N8 Zn2 126.3(6) . 2_546 ?
C11 N8 Zn2 121.9(7) . 2_546 ?
C3 N9 C12 104.9(7) . . ?
C3 N9 Zn1 130.6(7) . . ?
C12 N9 Zn1 124.4(5) . . ?
C3 N10 C14 103.8(7) . . ?
C3 N10 Zn2 132.0(7) . . ?
C14 N10 Zn2 124.1(7) . . ?
Zn3 O1 Zn2 150.8(6) . 4_575 ?
N8 C1 N7 111.7(7) . . ?
N8 C1 C15 125.0(8) . . ?
N7 C1 C15 123.2(8) . . ?
N3 C2 N4 112.0(9) . . ?
N3 C2 C6 123.6(8) . . ?
N4 C2 C6 124.4(8) . . ?
N9 C3 N10 114.5(8) . . ?
N9 C3 C7 123.1(8) . . ?
N10 C3 C7 122.5(8) . . ?
N1 C4 N2 110.8(7) . . ?
N1 C4 C19 125.3(7) . . ?
N2 C4 C19 124.0(7) . . ?
N5 C5 N6 111.2(6) . . ?
N5 C5 C20 126.5(8) . . ?
N6 C5 C20 122.3(8) . . ?
N6 C8 C9 108.9(6) . . ?
N5 C9 C8 106.5(7) . . ?
C16 C10 N2 107.2(7) . . ?
N8 C11 C13 107.8(7) . . ?
N9 C12 C14 107.3(8) . . ?
N7 C13 C11 109.4(7) . . ?
N10 C14 C12 109.5(9) . . ?
N1 C16 C10 107.4(7) . . ?
C18 C17 N4 106.6(9) . . ?
C17 C18 N3 109.4(10) . . ?
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 N7 2.030(8) . ?
Zn1 N9 2.034(8) . ?
Zn1 N4 2.043(8) . ?
Zn1 N5 2.038(8) . ?
Zn2 N10 2.004(7) . ?
Zn2 O1 2.010(9) 4_576 ?
Zn2 N1 2.044(8) 1_556 ?
Zn2 N8 2.060(10) 2_556 ?
Zn3 O1 1.997(10) . ?
Zn3 N2 2.027(7) . ?
Zn3 N6 2.030(9) 2_656 ?
Zn3 N3 2.048(8) . ?
N1 C4 1.352(9) . ?
N1 C16 1.376(10) . ?
N2 C4 1.370(9) . ?
N2 C10 1.398(10) . ?
N3 C2 1.333(10) . ?
N3 C18 1.381(13) . ?
N4 C2 1.362(10) . ?
N4 C17 1.372(12) . ?
N5 C5 1.334(10) . ?
N5 C9 1.354(9) . ?
N6 C5 1.357(10) . ?
N6 C8 1.379(10) . ?
N7 C13 1.378(9) . ?
N7 C1 1.374(10) . ?
N8 C1 1.357(10) . ?
N8 C11 1.374(9) . ?
N9 C3 1.346(9) . ?
N9 C12 1.390(12) . ?
N10 C3 1.354(10) . ?
N10 C14 1.381(12) . ?
C1 C15 1.501(10) . ?
C2 C6 1.499(12) . ?
C3 C7 1.503(12) . ?
C4 C19 1.507(10) . ?
C5 C20 1.494(9) . ?
C8 C9 1.389(12) . ?
C10 C16 1.414(10) . ?
C11 C13 1.381(12) . ?
C12 C14 1.396(10) . ?
C17 C18 1.384(11) . ?
