#------------------------------------------------------------------------------
#$Date: 2019-07-12 07:21:08 +0300 (Fri, 12 Jul 2019) $
#$Revision: 216970 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552093.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1552093
loop_
_publ_author_name
'Wang, Bin'
'Zou, Xiaodong'
'Smeets, Stef'
_publ_section_title
;
 Automated serial rotation electron diffraction combined with cluster
 analysis: an efficient multi-crystal workflow for structure determination
;
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252519007681
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C192 O96.16 Ti16 Zr4'
_chemical_formula_sum            'C192 O96.16 Ti16 Zr4'
_chemical_formula_weight         4975.28
_chemical_name_common            PCN-416
_chemical_name_systematic        PCN-416
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   16.5(4)
_cell_length_b                   16.5(4)
_cell_length_c                   29.8(8)
_cell_measurement_reflns_used    2825
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      1.80
_cell_measurement_theta_min      0.072
_cell_volume                     8113(4)
_computing_cell_refinement       'XDS-20180126 (Kabsch, 2018)'
_computing_data_collection       'Instamatic-1.0.0 (Smeets et al., 2018)'
_computing_data_reduction        'XDS-20180126 (Kabsch, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.2295
_diffrn_reflns_av_unetI/netI     0.2829
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11248
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        0.797
_diffrn_reflns_theta_max         0.797
_diffrn_reflns_theta_min         0.085
_diffrn_source                   'electron microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    1.020
_exptl_crystal_description       nano-crystals
_exptl_crystal_F_000             1010
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_coef       147(52)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.2785
_refine_ls_R_factor_gt           0.2163
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²+1.0000sinθ/λ] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4738
_refine_ls_wR_factor_ref         0.5351
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                1254
_reflns_number_total             2825
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fc5033.cif
_cod_data_source_block           PCN416
_cod_original_cell_volume        8086(480)
_cod_database_code               1552093
_shelx_shelxl_version_number     2014/7
_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'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+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'
'-x+1/2, y+1/2, -z+1/2'
'x+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'
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
Ti1 Ti 0.1083(4) 0.1083(4) 0.4427(3) 0.051(3) Uani 1 2 d S TU P
Ti2 Ti 0.1081(5) 0.1081(5) 0.5585(3) 0.067(3) Uani 1 2 d S TU P
Zr1 Zr 0.0000 0.0000 0.37713(18) 0.059(3) Uani 1 4 d S TU P
O1 O 0.0804(7) 0.0804(7) 0.4999(8) 0.049(4) Uani 1 2 d S TU P
O2 O -0.0013(14) 0.1089(9) 0.4194(4) 0.071(4) Uani 1 1 d . U .
O3 O 0.2292(12) 0.0871(16) 0.5353(8) 0.097(7) Uani 1 1 d D U .
O4 O 0.2250(11) 0.1162(14) 0.4591(7) 0.085(6) Uani 1 1 d D U .
O5 O 0.1568(14) 0.1568(14) 0.3790(7) 0.098(10) Uani 1 2 d DS TU P
O6 O 0.0763(13) 0.0763(13) 0.3358(8) 0.096(9) Uani 1 2 d DS TU P
O7 O 0.3501(17) 0.3501(17) 0.1143(9) 0.150(19) Uani 1 2 d DS TU P
O8 O 0.4232(14) 0.4232(14) 0.1643(9) 0.106(11) Uani 1 2 d DS TU P
C1 C 0.2620(11) 0.1066(19) 0.4977(8) 0.118(8) Uani 1 1 d D U .
C2 C 0.3500(12) 0.104(2) 0.4927(10) 0.173(12) Uani 1 1 d D U .
C3 C 0.4005(13) 0.103(3) 0.5310(10) 0.211(14) Uani 1 1 d D U .
C4 C 0.4840(11) 0.098(4) 0.5216(5) 0.226(15) Uani 1 1 d D U .
C5 C 0.5329(13) 0.092(4) 0.5605(9) 0.254(18) Uani 1 1 d D U .
C6 C 0.6165(15) 0.101(4) 0.5505(11) 0.28(2) Uani 1 1 d D U .
C7 C 0.1311(14) 0.1311(14) 0.3422(8) 0.149(17) Uani 1 2 d DS TU P
C8 C 0.1654(15) 0.1654(15) 0.3019(8) 0.176(15) Uani 1 2 d DS TU P
C9 C 0.1415(17) 0.1415(17) 0.2585(9) 0.203(18) Uani 1 2 d DS TU P
C10 C 0.1774(19) 0.1774(19) 0.2202(11) 0.246(19) Uani 1 2 d DS TU P
C11 C 0.2370(17) 0.2370(17) 0.2258(13) 0.225(16) Uani 1 2 d DS TU P
C12 C 0.2608(18) 0.2608(18) 0.2694(13) 0.232(17) Uani 1 2 d DS TU P
C13 C 0.2250(16) 0.2250(16) 0.3078(11) 0.214(18) Uani 1 2 d DS TU P
C14 C 0.321(2) 0.321(2) 0.2737(12) 0.25(2) Uani 1 2 d DS TU P
C15 C 0.355(2) 0.355(2) 0.2343(12) 0.23(2) Uani 1 2 d DS TU P
C16 C 0.3296(17) 0.3296(17) 0.1917(11) 0.190(16) Uani 1 2 d DS TU P
C17 C 0.2697(18) 0.2697(18) 0.1858(12) 0.205(18) Uani 1 2 d DS TU P
C18 C 0.3687(15) 0.3687(15) 0.1538(10) 0.161(18) Uani 1 2 d DS TU P
OW1 O 0.815(8) 0.958(8) 0.117(3) 0.25(8) Uiso 0.51(14) 1 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 4.3.2.2 and 4.3.2.3'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.3.2.2 and 4.3.2.3'
Ti Ti 0.0000 0.0000 'International Tables Vol C Tables 4.3.2.2 and 4.3.2.3'
Zr Zr 0.0000 0.0000 'International Tables Vol C Tables 4.3.2.2 and 4.3.2.3'
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 Ti1 O2 95.9(14) . .
O1 Ti1 O2 95.9(14) . 8
O2 Ti1 O2 83.2(11) . 8
O1 Ti1 O4 91.7(13) . 8
O2 Ti1 O4 98.3(9) . 8
O2 Ti1 O4 172.1(9) 8 8
O1 Ti1 O4 91.7(13) . .
O2 Ti1 O4 172.1(9) . .
O2 Ti1 O4 98.3(9) 8 .
O4 Ti1 O4 79.2(15) 8 .
O1 Ti2 O2 95.8(14) . 5_556
O1 Ti2 O2 95.8(14) . 3_556
O2 Ti2 O2 83.7(11) 5_556 3_556
O1 Ti2 O7 169.9(15) . 10
O2 Ti2 O7 91.7(17) 5_556 10
O2 Ti2 O7 91.7(17) 3_556 10
O1 Ti2 O3 83.4(13) . .
O2 Ti2 O3 171.0(10) 5_556 .
O2 Ti2 O3 87.4(10) 3_556 .
O7 Ti2 O3 90.2(16) 10 .
O1 Ti2 O3 83.4(13) . 8
O2 Ti2 O3 87.4(10) 5_556 8
O2 Ti2 O3 171.0(10) 3_556 8
O7 Ti2 O3 90.2(16) 10 8
O3 Ti2 O3 101.3(15) . 8
O6 Zr1 O6 111(3) 2 .
O6 Zr1 O8 71.1(11) 2 12_545
O6 Zr1 O8 71.1(11) . 12_545
O6 Zr1 O8 71.1(11) 2 11_455
O6 Zr1 O8 71.1(11) . 11_455
O8 Zr1 O8 111(3) 12_545 11_455
O6 Zr1 O2 142.9(8) 2 .
O6 Zr1 O2 81.8(18) . .
O8 Zr1 O2 143.9(8) 12_545 .
O8 Zr1 O2 81.1(18) 11_455 .
O6 Zr1 O2 142.9(8) 2 8
O6 Zr1 O2 81.8(18) . 8
O8 Zr1 O2 81.1(18) 12_545 8
O8 Zr1 O2 143.9(8) 11_455 8
O2 Zr1 O2 71.7(15) . 8
O6 Zr1 O2 81.8(18) 2 7
O6 Zr1 O2 142.9(8) . 7
O8 Zr1 O2 143.9(8) 12_545 7
O8 Zr1 O2 81.1(18) 11_455 7
O2 Zr1 O2 69.8(15) . 7
O2 Zr1 O2 110(2) 8 7
O6 Zr1 O2 81.8(18) 2 2
O6 Zr1 O2 142.9(8) . 2
O8 Zr1 O2 81.1(18) 12_545 2
O8 Zr1 O2 143.9(8) 11_455 2
O2 Zr1 O2 110(2) . 2
O2 Zr1 O2 69.8(15) 8 2
O2 Zr1 O2 71.7(15) 7 2
Ti1 O1 Ti2 138.9(17) . .
Ti2 O2 Ti1 138.4(16) 4_556 .
Ti2 O2 Zr1 101.8(11) 4_556 .
Ti1 O2 Zr1 101.1(11) . .
C1 O3 Ti2 129.3(16) . .
C1 O4 Ti1 131.1(16) . .
C7 O6 Zr1 137(2) . .
C18 O7 Ti2 129(3) . 10_554
O3 C1 O4 127(2) . .
O3 C1 C2 120(2) . .
O4 C1 C2 112(2) . .
C6 C2 C3 121(3) 5_656 .
C6 C2 C1 119(2) 5_656 .
C3 C2 C1 120(2) . .
C4 C3 C2 115(2) . .
C4 C4 C3 124(2) 5_656 .
C4 C4 C5 123(3) 5_656 .
C3 C4 C5 114(2) . .
C4 C5 C6 112(3) . .
C2 C6 C5 125(2) 5_656 .
O5 C7 O6 127(3) . .
O5 C7 C8 118(3) . .
O6 C7 C8 115(3) . .
C13 C8 C9 121(2) . .
C13 C8 C7 116(3) . .
C9 C8 C7 123(3) . .
C8 C9 C10 120(3) . .
C11 C10 C9 119(3) . .
C10 C11 C12 120(2) . .
C10 C11 C17 116(3) . .
C12 C11 C17 124(3) . .
C14 C12 C11 118(2) . .
C14 C12 C13 121(3) . .
C11 C12 C13 121(3) . .
C8 C13 C12 119(3) . .
C12 C14 C15 119(3) . .
C16 C15 C14 121(3) . .
C15 C16 C17 122(3) . .
C15 C16 C18 116(3) . .
C17 C16 C18 122(3) . .
C16 C17 C11 115(3) . .
O7 C18 O8 124(3) . .
O7 C18 C16 121(4) . .
O8 C18 C16 115(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O1 1.82(5) .
Ti1 O2 1.93(5) .
Ti1 O2 1.93(5) 8
Ti1 O4 1.99(5) 8
Ti1 O4 1.99(5) .
Ti2 O1 1.86(5) .
Ti2 O2 1.88(5) 5_556
Ti2 O2 1.88(5) 3_556
Ti2 O7 1.93(5) 10
Ti2 O3 2.14(6) .
Ti2 O3 2.14(6) 8
Zr1 O6 2.16(5) 2
Zr1 O6 2.16(5) .
Zr1 O8 2.17(5) 12_545
Zr1 O8 2.17(5) 11_455
Zr1 O2 2.19(5) .
Zr1 O2 2.19(5) 8
Zr1 O2 2.19(5) 7
Zr1 O2 2.19(5) 2
O2 Ti2 1.88(5) 4_556
O3 C1 1.28(3) .
O4 C1 1.31(4) .
O5 C7 1.25(4) .
O6 C7 1.29(4) .
O7 C18 1.25(4) .
O7 Ti2 1.93(5) 10_554
O8 C18 1.31(4) .
C1 C2 1.46(5) .
C2 C6 1.40(4) 5_656
C2 C3 1.41(4) .
C3 C4 1.41(4) .
C4 C4 1.39(4) 5_656
C4 C5 1.41(4) .
C5 C6 1.42(4) .
C6 C2 1.40(4) 5_656
C7 C8 1.44(4) .
C8 C13 1.40(4) .
C8 C9 1.41(4) .
C9 C10 1.42(4) .
C10 C11 1.40(4) .
C11 C12 1.41(4) .
C11 C17 1.41(4) .
C12 C14 1.40(5) .
C12 C13 1.42(4) .
C14 C15 1.42(4) .
C15 C16 1.40(4) .
C16 C17 1.41(4) .
C16 C18 1.45(4) .
