#------------------------------------------------------------------------------
#$Date: 2022-01-27 01:42:50 +0200 (Thu, 27 Jan 2022) $
#$Revision: 272261 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/43/7244304.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_7244304
loop_
_publ_author_name
'Cheplakova, Anastasia M.'
'Samsonenko, Denis G.'
'Lazarenko, Vladimir'
'Dorovatovskii, Pavel'
'Zubavichus, Yan'
'Khrustalev, Victor N.'
'Rakhmanova, Marianna I.'
'Fedin, Vladimir P.'
_publ_section_title
;
 Synthesis, supramolecular isomerism, and photoluminescence of
 scandium(III) complexes with tetrafluoroterephthalate ligand
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01689J
_journal_year                    2022
_chemical_formula_sum            'C16 H18 F8 K O17 Sc'
_chemical_formula_weight         718.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-01 deposited with the CCDC.	2022-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.9823(2)
_cell_length_b                   11.4355(4)
_cell_length_c                   48.3424(13)
_cell_measurement_reflns_used    10088
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.40
_cell_volume                     4965.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_unetI/netI     0.0077
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            10025
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.035
_diffrn_reflns_theta_min         2.914
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1542
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0221
_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)+(0.0350P)²+9.1272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1477
_reflns_number_total             1542
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01689j2.cif
_cod_data_source_block           sn987
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7244304
_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.
;
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.925
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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
Sc1 Sc 0.375000 0.875000 0.375000 0.00876(10) Uani 1 4 d S T P . .
K1 K 0.125000 0.625000 0.18571(8) 0.0165(3) Uani 0.5 2 d S TU P A 1
O1M O 0.55203(9) 0.99513(7) 0.38502(2) 0.01510(17) Uani 1 1 d D . . . .
H11M H 0.5834(17) 1.0075(14) 0.4015(2) 0.018 Uiso 1 1 d D U . . .
H12M H 0.6215(14) 1.0097(13) 0.3735(3) 0.018 Uiso 1 1 d D U . . .
O2M O 0.21341(11) 0.45282(8) 0.14883(2) 0.0236(2) Uani 1 1 d D . . . .
H21M H 0.215(2) 0.3873(10) 0.1573(3) 0.028 Uiso 1 1 d D U . . .
H22M H 0.149(3) 0.447(3) 0.1357(5) 0.028 Uiso 0.5 1 d D U P B 1
H23M H 0.204(4) 0.500(2) 0.1624(5) 0.028 Uiso 0.5 1 d D U P C 2
O1 O 0.30644(8) 0.79598(6) 0.33361(2) 0.01313(17) Uani 1 1 d . . . . .
O2 O 0.35695(9) 0.77793(7) 0.18764(2) 0.01553(17) Uani 1 1 d . . . . .
C1 C 0.375000 0.875000 0.32068(3) 0.0108(3) Uani 1 2 d S T P . .
C2 C 0.375000 0.875000 0.28962(3) 0.0108(3) Uani 1 2 d S T P . .
C3 C 0.26133(11) 0.82266(9) 0.27446(2) 0.0129(2) Uani 1 1 d . . . . .
C4 C 0.26198(11) 0.82313(9) 0.24580(2) 0.0136(2) Uani 1 1 d . . . . .
C5 C 0.375000 0.875000 0.23063(3) 0.0112(3) Uani 1 2 d S T P . .
C6 C 0.375000 0.875000 0.19900(3) 0.0113(3) Uani 1 2 d S T P A .
F1 F 0.14510(8) 0.77277(7) 0.28704(2) 0.02240(17) Uani 1 1 d . . . . .
F2 F 0.14597(8) 0.77361(7) 0.23264(2) 0.02453(18) Uani 1 1 d . . . . .
O1W O 0.125000 0.625000 0.1805(2) 0.022(2) Uani 0.5 2 d DS TU P D 2
H11W H 0.199(3) 0.650(3) 0.1901(6) 0.026 Uiso 0.5 1 d D U P E 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 '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
O1M Sc1 O1M 84.98(4) 2_565 3 ?
O1M Sc1 O1M 84.98(4) 4_565 . ?
O1M Sc1 O1M 100.85(4) 3 . ?
O1M Sc1 O1M 100.85(4) 2_565 4_565 ?
O1M Sc1 O1M 154.04(4) 3 4_565 ?
O1M Sc1 O1M 154.04(4) 2_565 . ?
O1M Sc1 O1 75.25(3) 2_565 . ?
O1M Sc1 O1 75.25(3) 3 4_565 ?
O1M Sc1 O1 75.25(3) 4_565 3 ?
O1M Sc1 O1 75.26(3) . 2_565 ?
O1M Sc1 O1 75.50(3) . 4_565 ?
O1M Sc1 O1 75.50(3) 3 2_565 ?
O1M Sc1 O1 75.50(3) 2_565 3 ?
O1M Sc1 O1 75.50(3) 4_565 . ?
O1M Sc1 O1 81.73(3) . 3 ?
O1M Sc1 O1 81.74(3) 2_565 4_565 ?
O1M Sc1 O1 81.74(3) 4_565 2_565 ?
O1M Sc1 O1 81.74(3) 3 . ?
O1M Sc1 O1 130.44(3) . . ?
O1M Sc1 O1 130.44(3) 2_565 2_565 ?
O1M Sc1 O1 130.44(3) 4_565 4_565 ?
O1M Sc1 O1 130.44(3) 3 3 ?
O1M Sc1 C1 77.019(19) . 3 ?
O1M Sc1 C1 77.022(19) 2_565 3 ?
O1M Sc1 C1 77.022(19) 4_565 . ?
O1M Sc1 C1 77.022(19) 3 . ?
O1M Sc1 C1 102.978(19) 2_565 . ?
O1M Sc1 C1 102.978(19) 4_565 3 ?
O1M Sc1 C1 102.978(19) 3 3 ?
O1M Sc1 C1 102.981(19) . . ?
O1 Sc1 O1 57.32(4) 2_565 . ?
O1 Sc1 O1 57.32(4) 4_565 3 ?
O1 Sc1 O1 133.30(4) 3 . ?
O1 Sc1 O1 133.30(4) 4_565 2_565 ?
O1 Sc1 O1 148.66(4) 3 2_565 ?
O1 Sc1 O1 148.66(4) 4_565 . ?
O1 Sc1 C1 28.657(18) . . ?
O1 Sc1 C1 28.658(18) 4_565 3 ?
O1 Sc1 C1 28.658(18) 3 3 ?
O1 Sc1 C1 28.659(18) 2_565 . ?
O1 Sc1 C1 151.342(18) 2_565 3 ?
O1 Sc1 C1 151.342(18) 4_565 . ?
O1 Sc1 C1 151.342(18) 3 . ?
O1 Sc1 C1 151.343(18) . 3 ?
C1 Sc1 C1 180.0 3 . ?
O2M K1 O2M 99.96(13) 14_455 . ?
O2M K1 F1 76.92(3) 14_455 21_565 ?
O2M K1 F1 76.93(3) . 22_655 ?
O2M K1 F1 142.31(5) . 21_565 ?
O2M K1 F1 142.31(5) 14_455 22_655 ?
O2M K1 F2 96.18(3) . 14_455 ?
O2M K1 F2 96.18(3) 14_455 . ?
O2M K1 F2 156.84(7) . . ?
O2M K1 F2 156.84(7) 14_455 14_455 ?
O2M K1 H11W 99(3) . 14_455 ?
O2M K1 H11W 102(3) 14_455 14_455 ?
O2 K1 O2M 77.58(5) . 14_455 ?
O2 K1 O2M 77.58(5) 14_455 . ?
O2 K1 O2M 105.01(7) . . ?
O2 K1 O2M 105.01(7) 14_455 14_455 ?
O2 K1 O2 176.08(17) 14_455 . ?
O2 K1 F1 67.42(4) . 22_655 ?
O2 K1 F1 67.42(4) 14_455 21_565 ?
O2 K1 F1 110.73(6) . 21_565 ?
O2 K1 F1 110.73(6) 14_455 22_655 ?
O2 K1 F2 62.46(5) . . ?
O2 K1 F2 62.46(5) 14_455 14_455 ?
O2 K1 F2 114.07(11) . 14_455 ?
O2 K1 F2 114.07(11) 14_455 . ?
O2 K1 H11W 22(3) 14_455 14_455 ?
O2 K1 H11W 155(3) . 14_455 ?
F1 K1 F1 127.88(14) 22_655 21_565 ?
F1 K1 H11W 47(3) 21_565 14_455 ?
F1 K1 H11W 116(3) 22_655 14_455 ?
F2 K1 F1 57.96(6) . 21_565 ?
F2 K1 F1 57.96(6) 14_455 22_655 ?
F2 K1 F1 80.14(8) . 22_655 ?
F2 K1 F1 80.14(8) 14_455 21_565 ?
F2 K1 F2 74.01(10) 14_455 . ?
F2 K1 H11W 59(3) 14_455 14_455 ?
F2 K1 H11W 93(3) . 14_455 ?
Sc1 O1M H11M 123.8(10) . . ?
Sc1 O1M H12M 121.1(10) . . ?
H11M O1M H12M 109.6(15) . . ?
K1 O2M H21M 108.6(11) . . ?
K1 O2M H22M 110(2) . . ?
H21M O2M H22M 107(2) . . ?
H21M O2M H23M 101(2) . . ?
C1 O1 Sc1 91.09(7) . . ?
C6 O2 K1 133.27(7) . . ?
O1 C1 Sc1 60.26(6) . . ?
O1 C1 Sc1 60.26(6) 2_565 . ?
O1 C1 O1 120.51(12) . 2_565 ?
O1 C1 C2 119.74(6) . . ?
O1 C1 C2 119.74(6) 2_565 . ?
C2 C1 Sc1 180.0 . . ?
C3 C2 C1 121.76(6) . . ?
C3 C2 C1 121.76(6) 2_565 . ?
C3 C2 C3 116.48(12) 2_565 . ?
C4 C3 C2 121.44(10) . . ?
F1 C3 C2 121.13(9) . . ?
F1 C3 C4 117.40(9) . . ?
C3 C4 C5 122.27(10) . . ?
F2 C4 C3 117.88(9) . . ?
F2 C4 C5 119.83(9) . . ?
C4 C5 C4 116.10(13) 2_565 . ?
C4 C5 C6 121.95(6) . . ?
C4 C5 C6 121.95(6) 2_565 . ?
O2 C6 O2 127.84(13) . 2_565 ?
O2 C6 C5 116.08(6) . . ?
O2 C6 C5 116.08(6) 2_565 . ?
C3 F1 K1 131.74(7) . 21_565 ?
C4 F2 K1 132.88(6) . . ?
H11W O1W H11W 114(5) . 14_455 ?
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
Sc1 O1M 2.1564(8) 2_565 ?
Sc1 O1M 2.1564(8) 3 ?
Sc1 O1M 2.1564(8) 4_565 ?
Sc1 O1M 2.1565(8) . yes
Sc1 O1 2.2802(7) 2_565 ?
Sc1 O1 2.2802(7) 3 ?
Sc1 O1 2.2802(7) 4_565 ?
Sc1 O1 2.2803(7) . yes
Sc1 C1 2.6256(13) 3 ?
Sc1 C1 2.6257(13) . yes
K1 O2M 2.772(3) . yes
K1 O2M 2.772(3) 14_455 ?
K1 O2 2.7217(8) . yes
K1 O2 2.7217(8) 14_455 ?
K1 F1 2.9980(19) 21_565 ?
K1 F1 2.9980(19) 22_655 ?
K1 F2 2.841(3) . yes
K1 F2 2.841(3) 14_455 ?
O1M H11M 0.856(9) . ?
O1M H12M 0.854(9) . ?
O2M H21M 0.853(9) . ?
O2M H22M 0.862(10) . ?
O2M H23M 0.854(10) . ?
O1 C1 1.2594(10) . ?
O2 C6 1.2490(10) . ?
C1 C2 1.5019(18) . ?
C2 C3 1.3920(12) . ?
C2 C3 1.3920(12) 2_565 ?
C3 C4 1.3856(14) . ?
C3 F1 1.3362(12) . ?
C4 C5 1.3858(12) . ?
C4 F2 1.3456(12) . ?
C5 C6 1.5291(18) . ?
O1W H11W 0.858(10) . ?
O1W H11W 0.858(10) 14_455 ?
