Synthesis, characterization and mass-spectrometric analysis of [LSn(IV)F<sub>4-x</sub>]<sup>x+</sup> salts [L = tris ((1-ethyl-benzoimidazol-2-yl)methyl)amine, x = 1-4].
Suter, Riccardo; Swidan, Ala'aeddeen; Zijlstra, Harmen S.; Macdonald, Charles L. B.; McIndoe, J. Scott; Burford, Neil; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16729–16736; doi:10.1039/c8dt03908a

data_7048015
_publ_section_title
;
 Synthesis, characterization and mass-spectrometric analysis of
 [LSn(IV)F<sub>4-x</sub>]<sup>x+</sup> salts [L = tris
 ((1-ethyl-benzoimidazol-2-yl)methyl)amine, x = 1-4].
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16729
_journal_page_last               16736
_journal_paper_doi               10.1039/c8dt03908a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'2(C32 H33 F6 N7 O6 S2 Sn), 4(C F3 O3 S), 0.5(C H2 Cl2), 0.5(C3 H6 N2)'
_chemical_formula_sum            'C70 H67 Cl F24 N15 O24 S8 Sn2'
_chemical_formula_weight         2487.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-26 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.119(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3317(12)
_cell_length_b                   17.1334(15)
_cell_length_c                   42.567(4)
_cell_measurement_reflns_used    9110
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      29.192
_cell_measurement_theta_min      2.937
_cell_volume                     9667.6(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       Bruker
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            145383
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.899
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0664 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.8945. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             4980
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.856
_refine_diff_density_min         -3.359
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1540
_refine_ls_number_reflns         18951
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.282
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0923
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+135.4464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17168
_reflns_number_total             18951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03908a2.cif
_cod_data_source_block           asrs11126_p21c
_cod_depositor_comments
'Adding full bibliography for 7048015--7048019.cif.'
_cod_original_cell_volume        9667.5(15)
_cod_database_code               7048015
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C71-N15'
 1.137 with sigma of 0.01
 C71-N15
 1.456 with sigma of 0.01
 N15-N15'
 2.593 with sigma of 0.02
 N12-C59 \\sim N12-C60'
 with sigma of 0.02
 C59-C60 \\sim C60'-C59'
 with sigma of 0.02
 N12-C60 \\sim N12-C59'
 with sigma of 0.04
 S1'-O1 \\sim S1-O1
 with sigma of 0.02
 S1'-O3' \\sim S1-O3
 with sigma of 0.02
 S1'-O2' \\sim S1-O2
 with sigma of 0.02
 S1'-C31 \\sim S1-C31'
 with sigma of 0.02
 F2'-C31 \\sim F2-C31'
 with sigma of 0.02
 F1'-C31 \\sim F1-C31'
 with sigma of 0.02
 F3'-C31 \\sim F3-C31'
 with sigma of 0.02
 S1'-F2' \\sim S1-F2
 with sigma of 0.04
 S1'-F1' \\sim S1-F1
 with sigma of 0.04
 S1'-F3' \\sim S1-F3
 with sigma of 0.04
 O1-O3' \\sim O1-O3
 with sigma of 0.04
 O1-O2' \\sim O1-O2
 with sigma of 0.04
 O1-C31 \\sim O1-C31'
 with sigma of 0.04
 O3'-O2' \\sim O3-O2
 with sigma of 0.04
 O3'-C31 \\sim O3-C31'
 with sigma of 0.04
 F2'-F1' \\sim F2-F1
 with sigma of 0.04
 F2'-F3' \\sim F2-F3
 with sigma of 0.04
 F1'-F3' \\sim F1-F3
 with sigma of 0.04
 O2'-C31 \\sim O2-C31'
 with sigma of 0.04
 C67'-F21' \\sim C67'-F19'
 with sigma of 0.02
 S7'-F21' \\sim S7'-F19'
 with sigma of 0.04
 S7'-O21 \\sim S7'-O20' \\sim S7'-O19
 with sigma of 0.02
 O21-O20' \\sim O20'-O19 \\sim O21-O19
 with sigma of 0.04
 C67'-O21 \\sim C67'-O20' \\sim C67'-O19
 with sigma of 0.04
 C67'-F21' \\sim C67-F20
 with sigma of 0.02
 C67'-F19' \\sim C67-F21
 with sigma of 0.02
 C67'-S7' \\sim C67-S7
 with sigma of 0.02
 C67'-F20' \\sim C67-F19
 with sigma of 0.02
 S7'-O21 \\sim S7-O21
 with sigma of 0.02
 S7'-O20' \\sim S7-O20
 with sigma of 0.02
 S7'-O19 \\sim S7-O19
 with sigma of 0.02
 C67'-O21 \\sim C67-O21
 with sigma of 0.04
 C67'-O20' \\sim C67-O20
 with sigma of 0.04
 C67'-O19 \\sim C67-O19
 with sigma of 0.04
 F21'-F19' \\sim F20-F21
 with sigma of 0.04
 F21'-S7' \\sim F20-S7
 with sigma of 0.04
 F21'-F20' \\sim F20-F19
 with sigma of 0.04
 F19'-S7' \\sim F21-S7
 with sigma of 0.04
 F19'-F20' \\sim F21-F19
 with sigma of 0.04
 S7'-F20' \\sim S7-F19
 with sigma of 0.04
 O21-O20' \\sim O21-O20
 with sigma of 0.04
 O20'-O19 \\sim O20-O19
 with sigma of 0.04
 S3'-O8' \\sim S3-O7
 with sigma of 0.02
 S3'-O9' \\sim S3-O9
 with sigma of 0.02
 S3'-O7' \\sim S3-O8
 with sigma of 0.02
 S3'-C33' \\sim S3-C33
 with sigma of 0.02
 F9'-C33' \\sim F7-C33
 with sigma of 0.02
 F8'-C33' \\sim F8-C33
 with sigma of 0.02
 F7'-C33' \\sim F9-C33
 with sigma of 0.02
 S3'-F9' \\sim S3-F7
 with sigma of 0.04
 S3'-F8' \\sim S3-F8
 with sigma of 0.04
 S3'-F7' \\sim S3-F9
 with sigma of 0.04
 F9'-F8' \\sim F7-F8
 with sigma of 0.04
 F9'-F7' \\sim F7-F9
 with sigma of 0.04
 O8'-O9' \\sim O7-O9
 with sigma of 0.04
 O8'-O7' \\sim O7-O8
 with sigma of 0.04
 O8'-C33' \\sim O7-C33
 with sigma of 0.04
 O9'-O7' \\sim O9-O8
 with sigma of 0.04
 O9'-C33' \\sim O9-C33
 with sigma of 0.04
 O7'-C33' \\sim O8-C33
 with sigma of 0.04
 F8'-F7' \\sim F8-F9
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C67' \\sim F21' \\sim F19' \\sim S7' \\sim O21 \\sim O20' \\sim O19: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
N15' \\sim C71 \\sim N15: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(N15) = Uanis(N15')
Uanis(C70) = Uanis(C70')
4. Rigid body (RIGU) restrains
 C67', F21', F19', S7', O21, O20', O19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, O7, O9, S3, C33, F9, F8, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F20, F21, C67, F19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N15, C70', C71, N15', C70
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C60')=Sof(H60D)=Sof(H60E)=Sof(C59')=Sof(H59C)=Sof(H59D)=Sof(H59E)=1-FVAR(1)
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
 Sof(F2)=Sof(F3)=Sof(C31')=Sof(F1)=Sof(S1)=Sof(O2)=Sof(O3)=1-FVAR(2)
 Sof(S1')=Sof(O3')=Sof(F2')=Sof(F1')=Sof(O2')=Sof(F3')=Sof(C31)=FVAR(2)
 Sof(F7)=Sof(F8)=Sof(C33)=Sof(F9)=Sof(S3)=Sof(O9)=Sof(O7)=Sof(O8)=1-FVAR(3)
 Sof(S3')=Sof(F9')=Sof(O8')=Sof(O9')=Sof(O7')=Sof(F8')=Sof(F7')=Sof(C33')=
 FVAR(3)
 Fixed Sof: C67'(0.75) F21'(0.75) F19'(0.75) S7'(0.75) O20'(0.75) Cl1(0.5)
 Cl0A(0.5) C69(0.5) H69A(0.5) H69B(0.5) F20'(0.75) F19(0.25) F21(0.25)
 C67(0.25) F20(0.25) O20(0.25) S7(0.25) N15'(0.5) C71(0.5) N15(0.5) C70'(0.5)
 H70A(0.5) H70B(0.5) H70C(0.5) C70(0.5) H70D(0.5) H70E(0.5) H70F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C27(H27A,H27B), C37(H37A,H37B), C39(H39A,H39B), C35(H35A,H35B),
 C3(H3A,H3B), C5(H5A,H5B), C25(H25A,H25B), C61(H61A,H61B), C63(H63A,H63B),
 C29(H29A,H29B), C59(H59A,H59B), C60'(H60D,H60E), C69(H69A,H69B)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C8(H8), C11(H11), C9(H9), C16(H16), C57(H57), C48(H48), C51(H51),
 C20(H20), C14(H14), C56(H56), C54(H54), C10(H10), C45(H45), C42(H42), C15(H15),
  C43(H43), C21(H21), C44(H44), C55(H55), C22(H22), C23(H23), C49(H49), C50(H50)
6.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C62(H62A,H62B,
 H62C), C64(H64A,H64B,H64C), C60(H60A,H60B,H60C), C59'(H59C,H59D,H59E),
 C70'(H70A,H70B,H70C), C70(H70D,H70E,H70F)
;
_shelx_res_checksum              58373
_olex2_submission_special_instructions 'No special instructions were received'