#------------------------------------------------------------------------------
#$Date: 2022-01-06 22:14:58 +0100 (jue 06 de ene de 2022) $
#$Revision: 271839 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/39/7243940.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_7243940
loop_
_publ_author_name
'Ito, Sho'
'White, Fraser J.'
'Okunishi, Eiji'
'Aoyama, Yoshitaka'
'Yamano, Akihito'
'Sato, Hiroyasu'
'Ferrara, Joseph D.'
'Jasnowski, Michał'
'Meyer, Mathias'
_publ_section_title
;
 Structure determination of small molecule compounds by an electron
 diffractometer for 3D ED/MicroED
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              8622
_journal_page_last               8630
_journal_paper_doi               10.1039/D1CE01172C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'Cl4 K2 Pt'
_chemical_formula_sum            'Cl4 K2 Pt'
_chemical_formula_weight         415.08
_space_group_crystal_system      tetragonal
_space_group_IT_number           123
_space_group_name_Hall           '-P 4 2'
_space_group_name_H-M_alt        'P 4/m m m'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-31 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   7.0688(11)
_cell_length_b                   7.0688(11)
_cell_length_c                   4.1570(16)
_cell_measurement_reflns_used    496
_cell_measurement_temperature    293
_cell_measurement_theta_max      0.9140
_cell_measurement_theta_min      0.1420
_cell_volume                     207.72(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.18a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.18a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.18a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Rigaku HyPix-ED area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -40.00  35.00   1.00   10.00    --    0.00   0.00   0.00   75
;
_diffrn_measurement_device       'Electron diffractometer'
_diffrn_measurement_device_type  Rigaku_Synergy-ED
_diffrn_measurement_method       'continuous rotation'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0001856000
_diffrn_orient_matrix_UB_12      -0.0029456000
_diffrn_orient_matrix_UB_13      0.0033448000
_diffrn_orient_matrix_UB_21      0.0035479000
_diffrn_orient_matrix_UB_22      -0.0001295000
_diffrn_orient_matrix_UB_23      0.0002388000
_diffrn_orient_matrix_UB_31      -0.0000357000
_diffrn_orient_matrix_UB_32      0.0019716000
_diffrn_orient_matrix_UB_33      0.0050249000
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200 keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.804
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            430
_diffrn_reflns_point_group_measured_fraction_full 0.804
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        0.859
_diffrn_reflns_theta_max         0.859
_diffrn_reflns_theta_min         0.144
_diffrn_source                   'thermionic-emission electron gun'
_diffrn_source_type              LaB6
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.18a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish red'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             48
_exptl_crystal_size_max          0.0003
_exptl_crystal_size_mid          0.0001
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       2303(40)
_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   3.167
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     11
_refine_ls_number_reflns         111
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      3.069
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.1652
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1400P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4466
_refine_ls_wR_factor_ref         0.4466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                111
_reflns_number_total             111
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01172c1.cif
_cod_data_source_block           exp_449
_cod_depositor_comments
'Adding full bibliography for 7243939--7243951.cif.'
_cod_original_cell_volume        207.72(10)
_cod_database_code               7243940
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K2 Pt Cl4'
_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.
;
_reflns_odcompleteness_completeness 84.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     0.86
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
K1 \\sim Pt3 \\sim Cl2: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
2. Rigid body (RIGU) restrains
 Pt3, Cl2, K1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
;
_shelx_res_file
;
TITL exp_449_a.res in P4/mmm
    exp_449.res
    created by SHELXL-2018/3 at 19:39:04 on 13-Jul-2021
REM Old TITL exp_449 in P4/mmm
REM SHELXT solution in P4/mmm: R1 0.211, Rweak 0.103, Alpha 0.063
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: Cl12 K6 Pt
CELL 0.0251 7.0688 7.0688 4.157 90 90 90
ZERR 1 0.0011 0.0011 0.0016 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SFAC  Cl 0.340 0.338 0.891 2.619 2.388 11.068 1.238 33.538 0 0 0 0 0.99 17
SFAC  K 0.566 0.506 2.415 5.766 2.466 31.917 3.524 151.259 0 0 0 0 1.96 19
SFAC  Pt 1.349 0.332 3.067 2.66 4.21 12.013 2.174 50.388 0 0 0 0 1.23 78
UNIT 4 2 1

RIGU 0.001 0.001 Pt3 Cl2 K1
SIMU 0.001 0.002 2 K1 Pt3 Cl2

L.S. 10 0 0
PLAN  2
SIZE 0.0003 0.0001 0.0001
TEMP 19.85
CONF
list 4
MORE -1
fmap 2 53
acta
OMIT 2 2 0
OMIT 4 4 0
OMIT 2 2 2
OMIT 1 1 1
OMIT 4 0 0
OMIT 2 0 0
OMIT 3 0 0
OMIT 4 0 2
OMIT 5 0 0
OMIT 3 3 3
OMIT 8 0 0
OMIT 4 3 1
OMIT 7 1 1
OMIT 6 2 1
OMIT 3 3 0
OMIT 7 3 0
REM <olex2.extras>
REM <HklSrc "%.\\exp_449.hkl">
REM </olex2.extras>

WGHT    0.140000
EXTI 2302.908203
FVAR       8.27785
PT3   3    0.500000    0.500000    0.500000    10.06250    0.00608    0.00608 =
         0.01500    0.00000    0.00000    0.00000
CL2   1    0.737025    0.262975    0.500000    10.25000    0.01334    0.01334 =
         0.01982    0.00000    0.00000    0.00622
K1    2    1.000000    0.500000    0.000000    10.12500    0.01833    0.04103 =
         0.00439    0.00000    0.00000    0.00000
HKLF 4




REM  exp_449_a.res in P4/mmm
REM wR2 = 0.4466, GooF = S = 3.167, Restrained GooF = 3.069 for all data
REM R1 = 0.1652 for 111 Fo > 4sig(Fo) and 0.1652 for all 111 data
REM 11 parameters refined using 9 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.532,  deepest hole -0.680,  1-sigma level  0.103
Q1    1   0.5000  0.5000  0.0000  10.06250  0.05    0.53
Q2    1   0.8620  0.1380  0.5000  10.25000  0.05    0.35
;
_shelx_res_checksum              16124
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.840
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, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, 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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt3 Pt 0.500000 0.500000 0.500000 0.009(4) Uani 1 16 d S T P . .
Cl2 Cl 0.7370(11) 0.2630(11) 0.500000 0.016(4) Uani 1 4 d S T P . .
K1 K 1.000000 0.500000 0.000000 0.021(5) Uani 1 8 d S T P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt3 0.006(4) 0.006(4) 0.015(6) 0.000 0.000 0.000
Cl2 0.013(5) 0.013(5) 0.020(9) 0.000 0.000 0.006(3)
K1 0.018(7) 0.041(10) 0.004(11) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt 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
Cl2 Pt3 Cl2 90.0 . 11_566 ?
Cl2 Pt3 Cl2 90.0 3_655 9_666 ?
Cl2 Pt3 Cl2 180.0 . 9_666 ?
Cl2 Pt3 Cl2 90.000(1) . 3_655 ?
Cl2 Pt3 Cl2 180.0 11_566 3_655 ?
Cl2 Pt3 Cl2 90.0 11_566 9_666 ?
Pt3 Cl2 K1 92.29(19) . 1_556 ?
Pt3 Cl2 K1 92.29(19) . 3_646 ?
Pt3 Cl2 K1 92.29(19) . 3_645 ?
Pt3 Cl2 K1 92.29(19) . . ?
K1 Cl2 K1 175.4(4) 1_556 3_645 ?
K1 Cl2 K1 175.4(4) . 3_646 ?
K1 Cl2 K1 100.39(3) 1_556 3_646 ?
K1 Cl2 K1 100.39(3) . 3_645 ?
K1 Cl2 K1 79.42(3) 1_556 . ?
K1 Cl2 K1 79.42(3) 3_645 3_646 ?
Cl2 K1 Cl2 110.3(3) 1_554 3_655 ?
Cl2 K1 Cl2 118.0(3) 1_554 11_666 ?
Cl2 K1 Cl2 62.0(3) 1_554 3_654 ?
Cl2 K1 Cl2 100.58(3) 11_666 3_655 ?
Cl2 K1 Cl2 110.3(3) . 3_654 ?
Cl2 K1 Cl2 118.0(3) . 11_665 ?
Cl2 K1 Cl2 62.0(3) . 3_655 ?
Cl2 K1 Cl2 69.7(3) 1_554 11_665 ?
Cl2 K1 Cl2 110.3(3) 9_765 11_666 ?
Cl2 K1 Cl2 79.42(3) 11_666 11_665 ?
Cl2 K1 Cl2 118.0(3) 9_766 3_654 ?
Cl2 K1 Cl2 180.0 3_655 11_665 ?
Cl2 K1 Cl2 69.7(3) 9_765 3_654 ?
Cl2 K1 Cl2 69.7(3) . 11_666 ?
Cl2 K1 Cl2 69.7(3) 9_766 3_655 ?
Cl2 K1 Cl2 62.0(3) 9_766 11_666 ?
Cl2 K1 Cl2 118.0(3) 9_765 3_655 ?
Cl2 K1 Cl2 100.58(3) . 9_766 ?
Cl2 K1 Cl2 79.42(3) 3_654 3_655 ?
Cl2 K1 Cl2 79.42(3) . 1_554 ?
Cl2 K1 Cl2 110.3(3) 9_766 11_665 ?
Cl2 K1 Cl2 180.0 9_766 1_554 ?
Cl2 K1 Cl2 62.0(3) 9_765 11_665 ?
Cl2 K1 Cl2 180.0 . 9_765 ?
Cl2 K1 Cl2 100.58(3) 3_654 11_665 ?
Cl2 K1 Cl2 79.42(3) 9_766 9_765 ?
Cl2 K1 Cl2 100.58(3) 1_554 9_765 ?
Cl2 K1 Cl2 180.0 11_666 3_654 ?
Cl2 K1 K1 50.289(13) . 1_556 ?
Cl2 K1 K1 129.711(13) 9_766 1_554 ?
Cl2 K1 K1 50.289(13) 3_654 1_554 ?
Cl2 K1 K1 50.289(13) 9_766 1_556 ?
Cl2 K1 K1 50.289(13) 9_765 1_554 ?
Cl2 K1 K1 129.711(13) 1_554 1_556 ?
Cl2 K1 K1 50.289(13) 11_665 1_554 ?
Cl2 K1 K1 129.711(13) 9_765 1_556 ?
Cl2 K1 K1 50.289(13) 1_554 1_554 ?
Cl2 K1 K1 50.289(13) 11_666 1_556 ?
Cl2 K1 K1 129.711(13) 11_666 1_554 ?
Cl2 K1 K1 129.711(14) 3_654 1_556 ?
Cl2 K1 K1 129.711(13) 3_655 1_554 ?
Cl2 K1 K1 50.289(13) 3_655 1_556 ?
Cl2 K1 K1 129.711(13) 11_665 1_556 ?
Cl2 K1 K1 129.711(13) . 1_554 ?
K1 K1 K1 180.0 1_556 1_554 ?
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
Pt3 Cl2 2.369(11) . ?
Pt3 Cl2 2.369(11) 3_655 ?
Pt3 Cl2 2.369(11) 11_566 ?
Pt3 Cl2 2.369(11) 9_666 ?
Cl2 K1 3.2531(7) . ?
Cl2 K1 3.2531(7) 3_646 ?
Cl2 K1 3.2531(7) 3_645 ?
Cl2 K1 3.2531(7) 1_556 ?
K1 K1 4.1570(16) 1_556 ?
K1 K1 4.1570(16) 1_554 ?
