#------------------------------------------------------------------------------
#$Date: 2021-02-16 21:59:27 +0200 (Tue, 16 Feb 2021) $
#$Revision: 262010 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/04/1560435.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_1560435
loop_
_publ_author_name
'Banihashemi, Fateme'
'Bu, Guanhong'
'Thaker, Amar'
'Williams, Dewight'
'Lin, Jerry Y S'
'Nannenga, Brent L'
_publ_section_title
;
 Beam-sensitive metal-organic framework structure determination by
 microcrystal electron diffraction.
;
_journal_name_full               Ultramicroscopy
_journal_page_first              113048
_journal_paper_doi               10.1016/j.ultramic.2020.113048
_journal_volume                  216
_journal_year                    2020
_chemical_formula_sum            'C96 H120 N48 Zn12'
_chemical_formula_weight         2730.91
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            1
_cell_length_a                   16.880(3)
_cell_length_b                   16.880(3)
_cell_length_c                   16.880(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4809.7(15)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_wavelength     1.000
_diffrn_reflns_av_R_equivalents  0.3206
_diffrn_reflns_av_unetI/netI     0.2108
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7484
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        34.949
_diffrn_reflns_theta_max         34.949
_diffrn_reflns_theta_min         3.396
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_F_000             483
_refine_diff_density_max         0.105
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_coef       0.07(3)
_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   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1779
_refine_ls_R_factor_gt           0.1348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1649P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3253
_refine_ls_wR_factor_ref         0.3411
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                342
_reflns_number_total             738
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            02-211_a.cif
_cod_data_source_block           02-211_a
_cod_original_cell_volume        4810(3)
_cod_database_code               1560435
_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, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+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 0.750000 0.500000 1.000000 0.072(3) Uani 1 4 d S T P . .
C1 C 0.6221(7) 0.3779(7) 1.0076(13) 0.086(6) Uani 1 2 d S T P . .
N1 N 0.6806(7) 0.4070(8) 0.9694(7) 0.082(4) Uani 1 1 d . . . . .
C2 C 0.6835(10) 0.3727(8) 0.9003(9) 0.110(5) Uani 1 1 d . . . . .
H1 H 0.717916 0.384863 0.858987 0.132 Uiso 1 1 calc R U . . .
C3 C 0.5948(9) 0.4052(9) 1.0842(12) 0.106(7) Uani 1 2 d S T P . .
H2A H 0.544104 0.430361 1.078378 0.160 Uiso 0.5 1 calc R U P . .
H2B H 0.632123 0.442480 1.105416 0.160 Uiso 0.5 1 calc R U P . .
H2C H 0.590037 0.360896 1.119486 0.160 Uiso 0.5 1 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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 109.5(4) 42_646 4_567
N1 Zn1 N1 109.3(7) 42_646 43_665
N1 Zn1 N1 109.5(4) 4_567 43_665
N1 Zn1 N1 109.5(4) 42_646 .
N1 Zn1 N1 109.3(7) 4_567 .
N1 Zn1 N1 109.5(4) 43_665 .
N1 C1 N1 109.9(19) . 14_665
N1 C1 C3 125.0(9) . .
N1 C1 C3 125.0(9) 14_665 .
C1 N1 C2 108.1(15) . .
C1 N1 Zn1 128.1(10) . .
C2 N1 Zn1 123.4(10) . .
N1 C2 C2 106.7(9) . 14_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.026(13) 42_646
Zn1 N1 2.026(13) 4_567
Zn1 N1 2.026(13) 43_665
Zn1 N1 2.026(13) .
C1 N1 1.277(13) .
C1 N1 1.277(13) 14_665
C1 C3 1.45(2) .
N1 C2 1.303(15) .
C2 C2 1.34(3) 14_665
