#------------------------------------------------------------------------------
#$Date: 2021-11-06 22:10:47 +0200 (Sat, 06 Nov 2021) $
#$Revision: 270454 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/24/1562403.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_1562403
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    3132
_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 0.537
_diffrn_measured_fraction_theta_max 0.530
_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  0.0886
_diffrn_reflns_av_unetI/netI     0.1100
_diffrn_reflns_Laue_measured_fraction_full 0.537
_diffrn_reflns_Laue_measured_fraction_max 0.530
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6502
_diffrn_reflns_point_group_measured_fraction_full 0.537
_diffrn_reflns_point_group_measured_fraction_max 0.530
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.935
_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         0.170
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       1313(17)
_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   1.950
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         3132
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.870
_refine_ls_R_factor_all          0.2192
_refine_ls_R_factor_gt           0.1784
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4033
_refine_ls_wR_factor_ref         0.4232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1874
_reflns_number_total             3132
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1fd00020a1.cif
_cod_data_source_block           5
_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               1562403
_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 0.2852(4) 0.37211(19) 0.7606(4) 0.0418(13) Uani 1 1 d . . . . .
Zn2 Zn 0.1223(5) 0.6473(2) 0.9751(5) 0.0518(18) Uani 1 1 d . . . . .
Zn3 Zn 0.2992(5) 0.6578(2) 0.4560(5) 0.0574(19) Uani 1 1 d . . . . .
N1 N 0.1996(13) 0.6137(6) 0.1338(12) 0.051(4) Uani 1 1 d D . . . .
N2 N 0.2543(13) 0.6163(6) 0.3070(12) 0.053(4) Uani 1 1 d D . . . .
N3 N 0.3312(14) 0.5526(7) 0.5547(13) 0.059(4) Uani 1 1 d D . . . .
N4 N 0.3354(12) 0.4537(6) 0.6765(11) 0.055(4) Uani 1 1 d D . . . .
N5 N 0.4113(11) 0.3126(6) 0.8893(11) 0.045(3) Uani 1 1 d D . . . .
N6 N 0.5575(12) 0.2285(6) 0.9905(11) 0.050(4) Uani 1 1 d D . . . .
N7 N 0.1865(14) 0.2752(6) 0.6590(13) 0.062(4) Uani 1 1 d D . . . .
N8 N 0.0416(14) 0.1824(7) 0.5754(13) 0.073(5) Uani 1 1 d D . . . .
N9 N 0.1888(12) 0.4447(6) 0.8070(12) 0.054(4) Uani 1 1 d D . . . .
N10 N 0.1324(12) 0.5467(6) 0.8892(13) 0.058(4) Uani 1 1 d D . . . .
O1 O 0.1729(14) 0.7321(7) 0.4471(13) 0.058(5) Uani 1 1 d . . . . .
C1 C 0.1106(11) 0.2232(6) 0.6659(11) 0.056(4) Uani 1 1 d D . . . .
C2 C 0.2738(12) 0.5050(6) 0.5914(11) 0.055(4) Uani 1 1 d D . . . .
C3 C 0.2180(11) 0.5109(6) 0.8789(10) 0.049(4) Uani 1 1 d D . . . .
C4 C 0.2147(11) 0.6657(6) 0.2175(11) 0.051(4) Uani 1 1 d D . . . .
C5 C 0.4948(11) 0.2644(7) 0.8938(11) 0.057(4) Uani 1 1 d D . . . .
C6 C 0.1498(16) 0.5083(9) 0.5399(18) 0.101(8) Uani 1 1 d D . . . .
C7 C 0.3336(15) 0.5410(9) 0.9417(16) 0.084(6) Uani 1 1 d D . . . .
C8 C 0.4997(15) 0.2495(8) 1.0431(14) 0.072(5) Uani 1 1 d D . . . .
C9 C 0.4126(14) 0.3017(8) 0.9844(13) 0.063(5) Uani 1 1 d D . . . .
C10 C 0.2583(14) 0.5278(7) 0.2735(14) 0.059(5) Uani 1 1 d D . . . .
C11 C 0.0822(16) 0.2033(9) 0.5077(15) 0.078(5) Uani 1 1 d D . . . .
C12 C 0.0753(14) 0.4373(7) 0.7652(14) 0.062(5) Uani 1 1 d D . . . .
C13 C 0.1681(14) 0.2616(8) 0.5563(13) 0.064(5) Uani 1 1 d D . . . .
C14 C 0.0427(14) 0.4997(7) 0.8153(14) 0.060(4) Uani 1 1 d D . . . .
C15 C 0.099(2) 0.2114(8) 0.7635(17) 0.097(8) Uani 1 1 d D . . . .
C16 C 0.2205(14) 0.5265(7) 0.1651(14) 0.058(5) Uani 1 1 d D . . . .
C17 C 0.4422(14) 0.4708(8) 0.7008(15) 0.080(5) Uani 1 1 d D . . . .
C18 C 0.4411(15) 0.5281(8) 0.6216(14) 0.065(5) Uani 1 1 d D . . . .
C19 C 0.1940(16) 0.7658(7) 0.2104(15) 0.067(7) Uani 1 1 d D . . . .
C20 C 0.5196(16) 0.2534(8) 0.8024(14) 0.057(4) 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 107.3(6) . . ?
N7 Zn1 N4 107.1(6) . . ?
N9 Zn1 N4 108.7(4) . . ?
N7 Zn1 N5 109.0(5) . . ?
N9 Zn1 N5 109.7(5) . . ?
N4 Zn1 N5 114.7(5) . . ?
N10 Zn2 O1 114.7(5) . 4_576 ?
N10 Zn2 N1 110.4(5) . 1_556 ?
O1 Zn2 N1 112.8(7) 4_576 1_556 ?
N10 Zn2 N8 110.7(7) . 2_556 ?
O1 Zn2 N8 96.8(6) 4_576 2_556 ?
N1 Zn2 N8 110.7(5) 1_556 2_556 ?
O1 Zn3 N2 106.2(7) . . ?
O1 Zn3 N6 112.6(5) . 2_656 ?
N2 Zn3 N6 108.5(5) . 2_656 ?
O1 Zn3 N3 111.8(5) . . ?
N2 Zn3 N3 110.9(5) . . ?
N6 Zn3 N3 106.8(7) 2_656 . ?
C4 N1 C16 109.6(12) . . ?
C4 N1 Zn2 128.1(8) . 1_554 ?
C16 N1 Zn2 120.9(10) . 1_554 ?
C4 N2 C10 104.6(12) . . ?
C4 N2 Zn3 128.3(8) . . ?
C10 N2 Zn3 127.1(10) . . ?
C2 N3 C18 103.3(12) . . ?
C2 N3 Zn3 135.8(12) . . ?
C18 N3 Zn3 119.5(8) . . ?
C2 N4 C17 105.2(10) . . ?
C2 N4 Zn1 129.2(10) . . ?
C17 N4 Zn1 125.5(10) . . ?
C5 N5 C9 106.4(11) . . ?
C5 N5 Zn1 128.5(9) . . ?
C9 N5 Zn1 124.2(8) . . ?
C5 N6 C8 102.9(12) . . ?
C5 N6 Zn3 128.8(7) . 2_646 ?
C8 N6 Zn3 128.3(11) . 2_646 ?
C13 N7 C1 103.6(11) . . ?
C13 N7 Zn1 125.9(8) . . ?
C1 N7 Zn1 129.4(9) . . ?
C1 N8 C11 104.3(12) . . ?
C1 N8 Zn2 127.3(8) . 2_546 ?
C11 N8 Zn2 123.2(14) . 2_546 ?
C3 N9 C12 105.0(9) . . ?
C3 N9 Zn1 129.4(10) . . ?
C12 N9 Zn1 125.6(8) . . ?
C3 N10 C14 102.4(10) . . ?
C3 N10 Zn2 132.9(11) . . ?
C14 N10 Zn2 124.5(9) . . ?
Zn3 O1 Zn2 147.0(8) . 4_575 ?
N8 C1 N7 114.3(11) . . ?
N8 C1 C15 121.0(12) . . ?
N7 C1 C15 124.7(13) . . ?
N3 C2 N4 115.3(13) . . ?
N3 C2 C6 121.7(13) . . ?
N4 C2 C6 122.9(10) . . ?
N9 C3 N10 114.5(12) . . ?
N9 C3 C7 122.5(10) . . ?
N10 C3 C7 123.0(12) . . ?
N1 C4 N2 110.5(10) . . ?
N1 C4 C19 124.0(11) . . ?
N2 C4 C19 125.5(11) . . ?
N5 C5 N6 112.4(11) . . ?
N5 C5 C20 124.0(12) . . ?
N6 C5 C20 123.6(11) . . ?
N6 C8 C9 111.3(13) . . ?
N5 C9 C8 106.6(10) . . ?
C16 C10 N2 109.8(11) . . ?
N8 C11 C13 109.0(13) . . ?
N9 C12 C14 107.1(12) . . ?
N7 C13 C11 108.5(10) . . ?
N10 C14 C12 111.0(13) . . ?
N1 C16 C10 105.3(11) . . ?
C18 C17 N4 107.8(14) . . ?
C17 C18 N3 108.1(12) . . ?
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 2.044(14) . ?
Zn1 N9 2.043(10) . ?
Zn1 N4 2.045(10) . ?
Zn1 N5 2.038(15) . ?
Zn2 N10 1.987(11) . ?
Zn2 O1 2.035(10) 4_576 ?
Zn2 N1 2.064(16) 1_556 ?
Zn2 N8 2.069(16) 2_556 ?
Zn3 O1 2.003(13) . ?
Zn3 N2 2.019(14) . ?
Zn3 N6 2.028(14) 2_656 ?
Zn3 N3 2.018(12) . ?
N1 C4 1.359(14) . ?
N1 C16 1.362(13) . ?
N2 C4 1.350(15) . ?
N2 C10 1.415(12) . ?
N3 C2 1.336(11) . ?
N3 C18 1.395(16) . ?
N4 C2 1.345(15) . ?
N4 C17 1.355(15) . ?
N5 C5 1.323(12) . ?
N5 C9 1.363(14) . ?
N6 C5 1.348(15) . ?
N6 C8 1.360(12) . ?
N7 C13 1.384(15) . ?
N7 C1 1.335(13) . ?
N8 C1 1.336(16) . ?
N8 C11 1.361(13) . ?
N9 C3 1.345(13) . ?
N9 C12 1.377(15) . ?
N10 C3 1.356(12) . ?
N10 C14 1.375(17) . ?
C1 C15 1.493(14) . ?
C2 C6 1.496(16) . ?
C3 C7 1.470(16) . ?
C4 C19 1.516(12) . ?
C5 C20 1.508(13) . ?
C8 C9 1.336(17) . ?
C10 C16 1.386(16) . ?
C11 C13 1.360(16) . ?
C12 C14 1.372(12) . ?
C17 C18 1.415(14) . ?
