#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:36:49 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289438 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/80/7248002.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_7248002
loop_
_publ_author_name
'Streit, Tim-Niclas'
'Gomila, Rosa M.'
'Sievers, Robin'
'Frontera, Antonio'
'Malischewski, Moritz'
_publ_section_title
;
 CF3-substituted sulfonium cations as efficient chalcogen bond donors
 towards cyanometalates
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              594
_journal_page_last               598
_journal_paper_doi               10.1039/D3CE01155K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C6 Mo N O5, C13 H6 F5 S, C H2 Cl2'
_chemical_formula_sum            'C20 H8 Cl2 F5 Mo N O5 S'
_chemical_formula_weight         636.17
_chemical_name_systematic        TNSUmeF2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-05 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.060(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1737(7)
_cell_length_b                   10.1525(3)
_cell_length_c                   25.8418(7)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.43
_cell_volume                     4768.0(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29494
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.346
_diffrn_reflns_theta_min         2.241
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6206
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0726 before and 0.0373 after correction.
The Ratio of minimum to maximum transmission is 0.8322.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_preparation
'Salt metathesis from Mo(CO)5CN NEt4 and UmeF2 Barf'
_exptl_crystal_size_max          0.714
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.527
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0462
_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)+(0.0001P)²+32.5442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5206
_reflns_number_total             5912
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01155k2.cif
_cod_data_source_block           c2c_forced
_cod_depositor_comments
'Adding full bibliography for 7248001--7248003.cif.'
_cod_database_code               7248002
_shelx_shelxl_version_number     2016/6
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C10(H10), C15(H15), C18(H18), C16(H16)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo01 Mo 0.59420(2) 0.14318(3) 0.42655(2) 0.02099(8) Uani 1 1 d . . . . .
S1 S 0.40118(4) 0.37834(8) 0.27718(3) 0.01783(16) Uani 1 1 d . . . . .
Cl1 Cl 0.54557(7) 0.67576(12) 0.30840(4) 0.0456(3) Uani 1 1 d . . . . .
Cl2 Cl 0.65873(8) 0.68408(16) 0.38786(6) 0.0654(4) Uani 1 1 d . . . . .
F3 F 0.25604(11) 0.3452(2) 0.26583(8) 0.0263(4) Uani 1 1 d . . . . .
F5 F 0.34686(13) -0.16528(19) 0.33505(9) 0.0303(5) Uani 1 1 d . . . . .
F2 F 0.29746(13) 0.5393(2) 0.24833(9) 0.0334(5) Uani 1 1 d . . . . .
F1 F 0.31536(12) 0.3792(3) 0.19537(8) 0.0367(6) Uani 1 1 d . . . . .
F4 F 0.32097(16) 0.4683(3) 0.49082(9) 0.0492(7) Uani 1 1 d . . . . .
O4 O 0.69649(16) -0.0029(3) 0.34567(10) 0.0391(7) Uani 1 1 d . . . . .
N1 N 0.52781(15) 0.3232(3) 0.32895(10) 0.0182(5) Uani 1 1 d . . . . .
O2 O 0.47810(17) -0.0876(3) 0.41017(11) 0.0377(7) Uani 1 1 d . . . . .
O5 O 0.73276(18) 0.3340(3) 0.43755(12) 0.0454(8) Uani 1 1 d . . . . .
O3 O 0.65344(18) -0.0401(3) 0.51581(11) 0.0401(7) Uani 1 1 d . . . . .
O1 O 0.4918(2) 0.3093(4) 0.50301(11) 0.0498(9) Uani 1 1 d . . . . .
C13 C 0.40249(18) 0.1072(3) 0.25491(12) 0.0185(6) Uani 1 1 d . . . . .
H13 H 0.421313 0.125157 0.221359 0.022 Uiso 1 1 calc R U . . .
C8 C 0.38726(17) 0.2074(3) 0.28942(12) 0.0157(6) Uani 1 1 d . . . . .
C12 C 0.38915(19) -0.0208(3) 0.27125(13) 0.0213(7) Uani 1 1 d . . . . .
H12 H 0.399348 -0.093573 0.249293 0.026 Uiso 1 1 calc R U . . .
C9 C 0.36010(18) 0.1869(3) 0.33936(12) 0.0170(6) Uani 1 1 d . . . . .
C10 C 0.34617(19) 0.0588(3) 0.35516(12) 0.0204(7) Uani 1 1 d . . . . .
H10 H 0.327418 0.040075 0.388659 0.025 Uiso 1 1 calc R U . . .
C1 C 0.54975(18) 0.2628(3) 0.36326(12) 0.0194(6) Uani 1 1 d . . . . .
C19 C 0.35391(19) 0.3093(3) 0.36908(12) 0.0196(6) Uani 1 1 d . . . . .
C15 C 0.3754(2) 0.5468(4) 0.36064(15) 0.0274(8) Uani 1 1 d . . . . .
H15 H 0.389242 0.619844 0.339873 0.033 Uiso 1 1 calc R U . . .
C14 C 0.37301(19) 0.4201(3) 0.34088(12) 0.0205(7) Uani 1 1 d . . . . .
C2 C 0.5170(2) -0.0007(4) 0.41590(13) 0.0270(8) Uani 1 1 d . . . . .
C11 C 0.36067(19) -0.0398(3) 0.32023(13) 0.0208(7) Uani 1 1 d . . . . .
C5 C 0.6814(2) 0.2717(4) 0.43498(14) 0.0299(8) Uani 1 1 d . . . . .
C7 C 0.31038(19) 0.4120(4) 0.24448(13) 0.0234(7) Uani 1 1 d . . . . .
C3 C 0.6327(2) 0.0285(4) 0.48374(13) 0.0280(8) Uani 1 1 d . . . . .
C4 C 0.6589(2) 0.0478(4) 0.37488(13) 0.0265(8) Uani 1 1 d . . . . .
C6 C 0.5279(2) 0.2491(4) 0.47614(14) 0.0325(9) Uani 1 1 d . . . . .
C17 C 0.3376(2) 0.4516(4) 0.44043(14) 0.0330(9) Uani 1 1 d . . . . .
C18 C 0.3348(2) 0.3251(4) 0.42080(13) 0.0266(8) Uani 1 1 d . . . . .
H18 H 0.320472 0.252385 0.441629 0.032 Uiso 1 1 calc R U . . .
C16 C 0.3564(2) 0.5615(4) 0.41220(16) 0.0346(9) Uani 1 1 d . . . . .
H16 H 0.356464 0.646166 0.427856 0.041 Uiso 1 1 calc R U . . .
C20 C 0.5706(2) 0.6292(4) 0.37202(14) 0.0346(9) Uani 1 1 d . . . . .
H20A H 0.534696 0.666549 0.396821 0.042 Uiso 1 1 calc R U . . .
H20B H 0.568714 0.532040 0.375036 0.042 Uiso 1 1 calc 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'
Cl Cl 0.1484 0.1585 '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'
Mo Mo -1.6832 0.6857 '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'
S S 0.1246 0.1234 '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
C2 Mo01 C1 92.46(13) . . ?
C2 Mo01 C5 173.18(15) . . ?
C2 Mo01 C6 93.14(16) . . ?
C5 Mo01 C1 90.62(14) . . ?
C3 Mo01 C1 178.02(15) . . ?
C3 Mo01 C2 85.59(15) . . ?
C3 Mo01 C5 91.28(16) . . ?
C3 Mo01 C4 90.34(15) . . ?
C3 Mo01 C6 92.75(15) . . ?
C4 Mo01 C1 89.25(13) . . ?
C4 Mo01 C2 88.21(15) . . ?
C4 Mo01 C5 85.74(15) . . ?
C4 Mo01 C6 176.71(15) . . ?
C6 Mo01 C1 87.69(13) . . ?
C6 Mo01 C5 93.07(16) . . ?
C8 S1 C7 97.56(16) . . ?
C14 S1 C8 91.55(15) . . ?
C14 S1 C7 96.85(15) . . ?
C8 C13 H13 121.4 . . ?
C8 C13 C12 117.2(3) . . ?
C12 C13 H13 121.4 . . ?
C13 C8 S1 125.0(2) . . ?
C13 C8 C9 123.9(3) . . ?
C9 C8 S1 111.0(2) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 C13 118.4(3) . . ?
C11 C12 H12 120.8 . . ?
C8 C9 C19 112.6(3) . . ?
C10 C9 C8 118.4(3) . . ?
C10 C9 C19 128.8(3) . . ?
C9 C10 H10 121.5 . . ?
C11 C10 C9 117.1(3) . . ?
C11 C10 H10 121.5 . . ?
N1 C1 Mo01 177.8(3) . . ?
C14 C19 C9 113.2(3) . . ?
C14 C19 C18 118.4(3) . . ?
C18 C19 C9 128.4(3) . . ?
C14 C15 H15 121.7 . . ?
C14 C15 C16 116.6(4) . . ?
C16 C15 H15 121.7 . . ?
C19 C14 S1 111.5(2) . . ?
C15 C14 S1 123.7(3) . . ?
C15 C14 C19 124.6(3) . . ?
O2 C2 Mo01 174.8(3) . . ?
F5 C11 C12 117.4(3) . . ?
F5 C11 C10 117.7(3) . . ?
C10 C11 C12 124.9(3) . . ?
O5 C5 Mo01 174.0(3) . . ?
F3 C7 S1 112.0(2) . . ?
F2 C7 S1 107.5(2) . . ?
F2 C7 F3 109.8(3) . . ?
F1 C7 S1 109.0(2) . . ?
F1 C7 F3 109.0(3) . . ?
F1 C7 F2 109.5(3) . . ?
O3 C3 Mo01 178.0(4) . . ?
O4 C4 Mo01 178.1(4) . . ?
O1 C6 Mo01 178.8(4) . . ?
F4 C17 C18 117.6(4) . . ?
F4 C17 C16 117.8(4) . . ?
C16 C17 C18 124.6(3) . . ?
C19 C18 H18 121.6 . . ?
C17 C18 C19 116.8(3) . . ?
C17 C18 H18 121.6 . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 119.0(3) . . ?
C17 C16 H16 120.5 . . ?
Cl1 C20 H20A 109.3 . . ?
Cl1 C20 H20B 109.3 . . ?
Cl2 C20 Cl1 111.6(2) . . ?
Cl2 C20 H20A 109.3 . . ?
Cl2 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
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
Mo01 C1 2.191(3) . ?
Mo01 C2 2.044(4) . ?
Mo01 C5 2.064(4) . ?
Mo01 C3 2.006(4) . ?
Mo01 C4 2.027(4) . ?
Mo01 C6 2.062(4) . ?
S1 C8 1.783(3) . ?
S1 C14 1.776(3) . ?
S1 C7 1.884(4) . ?
Cl1 C20 1.769(4) . ?
Cl2 C20 1.745(5) . ?
F3 C7 1.319(4) . ?
F5 C11 1.354(4) . ?
F2 C7 1.317(4) . ?
F1 C7 1.315(4) . ?
F4 C17 1.348(4) . ?
O4 C4 1.141(4) . ?
N1 C1 1.149(4) . ?
O2 C2 1.140(5) . ?
O5 C5 1.129(5) . ?
O3 C3 1.146(4) . ?
O1 C6 1.134(5) . ?
C13 H13 0.9500 . ?
C13 C8 1.381(4) . ?
C13 C12 1.388(5) . ?
C8 C9 1.398(4) . ?
C12 H12 0.9500 . ?
C12 C11 1.382(5) . ?
C9 C10 1.386(5) . ?
C9 C19 1.466(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.374(5) . ?
C19 C14 1.385(5) . ?
C19 C18 1.390(4) . ?
C15 H15 0.9500 . ?
C15 C14 1.384(5) . ?
C15 C16 1.385(5) . ?
C17 C18 1.382(5) . ?
C17 C16 1.376(6) . ?
C18 H18 0.9500 . ?
C16 H16 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
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
S1 C8 C9 C10 180.0(3) . . . . ?
S1 C8 C9 C19 -2.9(4) . . . . ?
F4 C17 C18 C19 -178.5(3) . . . . ?
F4 C17 C16 C15 178.6(4) . . . . ?
C13 C8 C9 C10 -1.3(5) . . . . ?
C13 C8 C9 C19 175.8(3) . . . . ?
C13 C12 C11 F5 178.9(3) . . . . ?
C13 C12 C11 C10 -1.9(5) . . . . ?
C8 S1 C14 C19 -0.4(3) . . . . ?
C8 S1 C14 C15 175.1(3) . . . . ?
C8 S1 C7 F3 37.4(3) . . . . ?
C8 S1 C7 F2 158.1(2) . . . . ?
C8 S1 C7 F1 -83.4(3) . . . . ?
C8 C13 C12 C11 1.0(5) . . . . ?
C8 C9 C10 C11 0.4(5) . . . . ?
C8 C9 C19 C14 2.7(4) . . . . ?
C8 C9 C19 C18 -174.4(3) . . . . ?
C12 C13 C8 S1 179.1(3) . . . . ?
C12 C13 C8 C9 0.5(5) . . . . ?
C9 C10 C11 F5 -179.6(3) . . . . ?
C9 C10 C11 C12 1.2(5) . . . . ?
C9 C19 C14 S1 -1.2(4) . . . . ?
C9 C19 C14 C15 -176.7(3) . . . . ?
C9 C19 C18 C17 175.9(3) . . . . ?
C10 C9 C19 C14 179.4(3) . . . . ?
C10 C9 C19 C18 2.3(6) . . . . ?
C19 C9 C10 C11 -176.2(3) . . . . ?
C14 S1 C8 C13 -176.8(3) . . . . ?
C14 S1 C8 C9 1.9(3) . . . . ?
C14 S1 C7 F3 -55.1(3) . . . . ?
C14 S1 C7 F2 65.6(3) . . . . ?
C14 S1 C7 F1 -175.9(3) . . . . ?
C14 C19 C18 C17 -1.1(5) . . . . ?
C14 C15 C16 C17 0.7(6) . . . . ?
C7 S1 C8 C13 86.1(3) . . . . ?
C7 S1 C8 C9 -95.2(3) . . . . ?
C7 S1 C14 C19 97.4(3) . . . . ?
C7 S1 C14 C15 -87.1(3) . . . . ?
C18 C19 C14 S1 176.2(3) . . . . ?
C18 C19 C14 C15 0.8(5) . . . . ?
C18 C17 C16 C15 -1.2(6) . . . . ?
C16 C15 C14 S1 -175.5(3) . . . . ?
C16 C15 C14 C19 -0.6(6) . . . . ?
C16 C17 C18 C19 1.4(6) . . . . ?
