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#$Date: 2023-04-04 13:11:49 +0300 (Tue, 04 Apr 2023) $
#$Revision: 282324 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/63/7246349.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_7246349
loop_
_publ_author_name
'Bogdan, Marta'
'Sierański, Tomasz'
'Świątkowski, Marcin'
'Trzęsowska-Kruszyńska, Agata'
_publ_section_title
;
 On structural factors determining the nature of the fluorescent
 properties of OIHMs based on 8-hydroxyquinoline
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1993
_journal_page_last               2002
_journal_paper_doi               10.1039/D3CE00061C
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         '2(C9 H8 N O), Cl6 Sn, 2(H2 O)'
_chemical_formula_sum            'C18 H20 Cl6 N2 O4 Sn'
_chemical_formula_weight         659.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                83.177(3)
_cell_angle_beta                 71.049(4)
_cell_angle_gamma                79.945(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2163(3)
_cell_length_b                   9.5228(4)
_cell_length_c                   9.5411(4)
_cell_measurement_reflns_used    10736
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.8800
_cell_measurement_theta_min      3.9450
_cell_volume                     609.24(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics
;XP in SHELXTL (Sheldrick, 2008)
 ORTEP-3 W v. 1.062 (Farrugia 2012)
;
_computing_publication_material
;SHELXL-2018/1 (Sheldrick, 2018) and
 PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            31869
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         3.455
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       needle
_exptl_crystal_F_000             326
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         4468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0383P)²+3.4367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4031
_reflns_number_total             4468
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce00061c2.cif
_cod_data_source_block           mz1084a
_cod_depositor_comments
'Adding full bibliography for 7246339--7246352.cif.'
_cod_database_code               7246349
_shelx_shelxl_version_number     2018/1
_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'
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
Sn1 Sn 0.500000 0.000000 0.500000 0.01197(19) Uani 1 2 d S . P . .
Cl1 Cl 0.4799(2) 0.25828(15) 0.50203(16) 0.0177(3) Uani 1 1 d . . . . .
Cl2 Cl 0.3610(2) 0.03174(17) 0.29663(16) 0.0194(3) Uani 1 1 d . . . . .
Cl3 Cl 0.1680(2) 0.01186(16) 0.67691(16) 0.0182(3) Uani 1 1 d . . . . .
O1 O 0.9080(8) 0.4547(5) 0.6454(5) 0.0246(11) Uani 1 1 d . . . . .
H1O H 0.915697 0.390181 0.590043 0.037 Uiso 1 1 calc R U . . .
N1 N 0.8622(7) 0.6411(6) 0.8449(6) 0.0161(11) Uani 1 1 d . . . . .
H1N H 0.908391 0.661678 0.748636 0.019 Uiso 1 1 d R U . . .
C1 C 0.8465(9) 0.7405(7) 0.9371(7) 0.0176(13) Uani 1 1 d . . . . .
H1 H 0.889812 0.829985 0.898425 0.021 Uiso 1 1 calc R U . . .
C2 C 0.7671(9) 0.7136(7) 1.0894(7) 0.0204(13) Uani 1 1 d . . . . .
H2 H 0.756037 0.784384 1.155014 0.025 Uiso 1 1 calc R U . . .
C3 C 0.7046(9) 0.5841(7) 1.1447(7) 0.0194(13) Uani 1 1 d . . . . .
H3 H 0.650163 0.566079 1.248957 0.023 Uiso 1 1 calc R U . . .
C6 C 0.6857(9) 0.2444(7) 0.9924(7) 0.0187(13) Uani 1 1 d . . . . .
H6 H 0.646997 0.152696 1.025112 0.022 Uiso 1 1 calc R U . . .
C5 C 0.6617(9) 0.3399(7) 1.0952(7) 0.0200(13) Uani 1 1 d . . . . .
H5 H 0.606083 0.314433 1.197946 0.024 Uiso 1 1 calc R U . . .
C4 C 0.7200(9) 0.4772(7) 1.0486(7) 0.0174(13) Uani 1 1 d . . . . .
C7 C 0.7663(9) 0.2786(7) 0.8387(7) 0.0180(13) Uani 1 1 d . . . . .
H7 H 0.779799 0.210341 0.769773 0.022 Uiso 1 1 calc R U . . .
C9 C 0.8019(9) 0.5102(7) 0.8932(7) 0.0156(12) Uani 1 1 d . . . . .
C8 C 0.8256(9) 0.4101(7) 0.7881(7) 0.0165(12) Uani 1 1 d . . . . .
O99 O 0.9508(7) 0.2570(5) 0.4532(5) 0.0196(9) Uani 1 1 d . . . . .
H99O H 1.046617 0.185203 0.463718 0.029 Uiso 1 1 d R U . . .
H99B H 0.857173 0.214843 0.440741 0.029 Uiso 1 1 d R U . . .
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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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 Sn1 Cl2 180.0 2_656 . ?
Cl2 Sn1 Cl3 89.90(5) 2_656 2_656 ?
Cl2 Sn1 Cl3 90.10(5) . 2_656 ?
Cl2 Sn1 Cl3 90.10(5) 2_656 . ?
Cl2 Sn1 Cl3 89.91(5) . . ?
Cl3 Sn1 Cl3 180.0 2_656 . ?
Cl2 Sn1 Cl1 89.35(5) 2_656 . ?
Cl2 Sn1 Cl1 90.66(5) . . ?
Cl3 Sn1 Cl1 90.25(5) 2_656 . ?
Cl3 Sn1 Cl1 89.75(5) . . ?
Cl2 Sn1 Cl1 90.66(5) 2_656 2_656 ?
Cl2 Sn1 Cl1 89.34(5) . 2_656 ?
Cl3 Sn1 Cl1 89.75(5) 2_656 2_656 ?
Cl3 Sn1 Cl1 90.25(5) . 2_656 ?
Cl1 Sn1 Cl1 180.0 . 2_656 ?
C8 O1 H1O 109.5 . . ?
C1 N1 C9 122.9(6) . . ?
C1 N1 H1N 118.7 . . ?
C9 N1 H1N 118.3 . . ?
N1 C1 C2 120.1(6) . . ?
N1 C1 H1 119.9 . . ?
C2 C1 H1 119.9 . . ?
C3 C2 C1 119.7(6) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 121.0(6) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C6 C7 121.7(6) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C5 C4 120.0(6) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C3 C4 C5 125.1(6) . . ?
C3 C4 C9 117.2(6) . . ?
C5 C4 C9 117.7(6) . . ?
C8 C7 C6 120.4(6) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
N1 C9 C8 119.4(6) . . ?
N1 C9 C4 119.1(6) . . ?
C8 C9 C4 121.5(6) . . ?
O1 C8 C7 126.3(6) . . ?
O1 C8 C9 115.2(5) . . ?
C7 C8 C9 118.6(6) . . ?
H99O O99 H99B 105.6 . . ?
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
Sn1 Cl2 2.4249(14) 2_656 ?
Sn1 Cl2 2.4249(14) . ?
Sn1 Cl3 2.4343(14) 2_656 ?
Sn1 Cl3 2.4343(14) . ?
Sn1 Cl1 2.4404(14) . ?
Sn1 Cl1 2.4405(14) 2_656 ?
O1 C8 1.347(7) . ?
O1 H1O 0.8400 . ?
N1 C1 1.333(8) . ?
N1 C9 1.371(8) . ?
N1 H1N 0.8802 . ?
C1 C2 1.388(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.374(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.416(9) . ?
C3 H3 0.9500 . ?
C6 C5 1.366(9) . ?
C6 C7 1.412(9) . ?
C6 H6 0.9500 . ?
C5 C4 1.420(9) . ?
C5 H5 0.9500 . ?
C4 C9 1.425(9) . ?
C7 C8 1.376(9) . ?
C7 H7 0.9500 . ?
C9 C8 1.415(9) . ?
O99 H99O 0.9052 . ?
O99 H99B 0.8885 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C1 C2 0.3(9) . . . . ?
N1 C1 C2 C3 -0.1(9) . . . . ?
C1 C2 C3 C4 0.1(9) . . . . ?
C7 C6 C5 C4 -0.5(9) . . . . ?
C2 C3 C4 C5 179.2(6) . . . . ?
C2 C3 C4 C9 -0.3(9) . . . . ?
C6 C5 C4 C3 -179.3(6) . . . . ?
C6 C5 C4 C9 0.3(9) . . . . ?
C5 C6 C7 C8 0.7(10) . . . . ?
C1 N1 C9 C8 -179.4(6) . . . . ?
C1 N1 C9 C4 -0.5(9) . . . . ?
C3 C4 C9 N1 0.5(8) . . . . ?
C5 C4 C9 N1 -179.1(5) . . . . ?
C3 C4 C9 C8 179.3(6) . . . . ?
C5 C4 C9 C8 -0.3(9) . . . . ?
C6 C7 C8 O1 178.6(6) . . . . ?
C6 C7 C8 C9 -0.7(9) . . . . ?
N1 C9 C8 O1 -0.1(8) . . . . ?
C4 C9 C8 O1 -178.9(5) . . . . ?
N1 C9 C8 C7 179.3(6) . . . . ?
C4 C9 C8 C7 0.5(9) . . . . ?
