#------------------------------------------------------------------------------
#$Date: 2019-07-12 07:21:08 +0300 (Fri, 12 Jul 2019) $
#$Revision: 216970 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552090.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_1552090
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         'O128 Si64'
_chemical_formula_sum            'O128 Si64'
_chemical_formula_weight         3845.38
_chemical_name_common            Mordenite
_chemical_name_systematic        Si-MOR
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c 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                   18.120
_cell_length_b                   20.000
_cell_length_c                   7.700
_cell_measurement_reflns_used    904
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      1.80
_cell_measurement_theta_min      0.072
_cell_volume                     2790.480
_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 0.570
_diffrn_measured_fraction_theta_max 0.549
_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  0.1014
_diffrn_reflns_av_unetI/netI     0.1620
_diffrn_reflns_Laue_measured_fraction_full 0.570
_diffrn_reflns_Laue_measured_fraction_max 0.549
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1941
_diffrn_reflns_point_group_measured_fraction_full 0.570
_diffrn_reflns_point_group_measured_fraction_max 0.549
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.911
_diffrn_reflns_theta_min         0.118
_diffrn_source                   'electron microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             626
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       9988(43)
_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   2.159
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.159
_refine_ls_R_factor_all          0.3181
_refine_ls_R_factor_gt           0.2910
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_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          0.6105
_refine_ls_wR_factor_ref         0.6472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                555
_reflns_number_total             904
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fc5033.cif
_cod_data_source_block           mordenite_mixed_phase
_cod_original_cell_volume        2790.5
_cod_database_code               1552090
_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+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-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'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'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'
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_occupancy
Si1 Si 0.9146(5) 0.7232(4) 0.7500 0.051(3) Uiso 1 2 d S P
Si2 Si 0.8042(4) 0.6891(3) 0.4570(12) 0.045(2) Uiso 1 1 d . .
Si3 Si 0.6946(4) 0.5743(3) 0.5406(11) 0.046(2) Uiso 1 1 d . .
Si4 Si 0.5845(6) 0.6203(4) 0.2500 0.051(3) Uiso 1 2 d S P
O1 O 0.5000 0.5960(10) 0.2500 0.056(5) Uiso 1 4 d S P
O2 O 1.0000 0.6966(9) 0.7500 0.063(6) Uiso 1 4 d S P
O3 O 0.7229(11) 0.5000 0.5000 0.074(5) Uiso 1 2 d S P
O4 O 0.7595(10) 0.6228(7) 0.493(3) 0.087(5) Uiso 1 1 d . .
O5 O 0.8295(12) 0.6916(8) 0.2500 0.078(6) Uiso 1 2 d S P
O6 O 0.6739(11) 0.5824(9) 0.7500 0.081(6) Uiso 1 2 d S P
O7 O 0.7500 0.7500 0.5000 0.085(6) Uiso 1 2 d S P
O8 O 0.8750(9) 0.6930(6) 0.577(2) 0.068(4) Uiso 1 1 d . .
O9 O 0.9057(14) 0.8014(8) 0.7500 0.085(6) Uiso 1 2 d S P
O10 O 0.6250(9) 0.5895(7) 0.422(2) 0.082(4) Uiso 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 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'
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
O9 Si1 O8 108.9(7) . .
O9 Si1 O8 108.9(7) . 10_557
O8 Si1 O8 109.8(12) . 10_557
O9 Si1 O2 114.9(12) . .
O8 Si1 O2 107.2(7) . .
O8 Si1 O2 107.2(7) 10_557 .
O4 Si2 O8 110.9(9) . .
O4 Si2 O7 106.7(8) . .
O8 Si2 O7 109.9(6) . .
O4 Si2 O5 109.6(9) . .
O8 Si2 O5 109.5(10) . .
O7 Si2 O5 110.2(7) . .
O4 Si3 O10 110.1(10) . .
O4 Si3 O3 106.7(9) . .
O10 Si3 O3 108.6(8) . .
O4 Si3 O6 109.6(10) . .
O10 Si3 O6 111.1(9) . .
O3 Si3 O6 110.6(7) . .
O9 Si4 O1 114.1(12) 13_666 .
O9 Si4 O10 109.0(7) 13_666 10_556
O1 Si4 O10 108.2(7) . 10_556
O9 Si4 O10 109.0(7) 13_666 .
O1 Si4 O10 108.2(7) . .
O10 Si4 O10 108.2(12) 10_556 .
Si4 O1 Si4 144.7(15) . 3_655
Si1 O2 Si1 142.0(14) . 3_756
Si3 O3 Si3 142.6(14) . 4_566
Si3 O4 Si2 161.1(12) . .
Si2 O5 Si2 147.7(16) . 10_556
Si3 O6 Si3 151.6(14) . 10_557
Si2 O7 Si2 180.0(3) 13_666 .
Si2 O8 Si1 148.4(11) . .
Si1 O9 Si4 167.6(17) . 13_666
Si3 O10 Si4 153.5(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O9 1.573(16) .
Si1 O8 1.631(16) .
Si1 O8 1.631(16) 10_557
Si1 O2 1.637(11) .
Si2 O4 1.578(18) .
Si2 O8 1.582(16) .
Si2 O7 1.600(7) .
Si2 O5 1.660(10) .
Si3 O4 1.569(17) .
Si3 O10 1.587(17) .
Si3 O3 1.603(10) .
Si3 O6 1.663(9) .
Si4 O9 1.574(17) 13_666
Si4 O1 1.607(11) .
Si4 O10 1.635(17) 10_556
Si4 O10 1.635(17) .
O1 Si4 1.607(11) 3_655
O2 Si1 1.637(11) 3_756
O3 Si3 1.603(10) 4_566
O5 Si2 1.660(10) 10_556
O6 Si3 1.663(9) 10_557
O7 Si2 1.600(7) 13_666
O9 Si4 1.574(17) 13_666
