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_7048016
_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         'C36 H48 F N7 O P Sn, 3(C F3 O3 S)'
_chemical_formula_sum            'C39 H48 F10 N7 O10 P S3 Sn'
_chemical_formula_weight         1210.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                81.027(3)
_cell_angle_beta                 71.795(2)
_cell_angle_gamma                62.150(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9482(10)
_cell_length_b                   13.7454(10)
_cell_length_c                   17.4270(13)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.227
_cell_measurement_theta_min      2.961
_cell_volume                     2604.9(3)
_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 0.999
_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  0.0736
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            84181
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.483
_diffrn_reflns_theta_min         2.961
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0618 before and 0.0551 after correction. The Ratio of minimum to maximum transmission is 0.9318. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       prism
_exptl_crystal_F_000             1228
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         10745
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0473
_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/[\s^2^(Fo^2^)+(0.0581P)^2^+5.3211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8615
_reflns_number_total             10745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03908a2.cif
_cod_data_source_block           asrs11140
_cod_depositor_comments
'Adding full bibliography for 7048015--7048019.cif.'
_cod_database_code               7048016
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.867
_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
 N6-C27' \\sim N6-C27
 with sigma of 0.02
 C27'-C28' \\sim C27-C28
 with sigma of 0.02
 N6-C28' \\sim N6-C28
 with sigma of 0.04
 C33-F9 \\sim C33-F10 \\sim C33-F8
 with sigma of 0.02
 F9-F10 \\sim F10-F8 \\sim F8-F9
 with sigma of 0.04
 S3-F9 \\sim S3-F10 \\sim S3-F8
 with sigma of 0.04
 S3-O8 \\sim S3-O10 \\sim S3-O9
 with sigma of 0.02
 O8-O10 \\sim O10-O9 \\sim O8-O9
 with sigma of 0.04
 C33-O8 \\sim C33-O10 \\sim C33-O9
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C33 \\sim F9 \\sim F10 \\sim F8 \\sim S3 \\sim O8 \\sim O10 \\sim O9: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C33, F9, F10, F8, S3, O8, O10, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C27'(0.78) H27a(0.78) H27b(0.78) C28'(0.78) H28a(0.78) H28b(0.78)
 H28c(0.78) C28(0.22) H28d(0.22) H28e(0.22) H28f(0.22) C27(0.22) H27c(0.22)
 H27d(0.22)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C3(H3a,H3b), C1(H1a,H1b), C29(H29a,H29b), C25(H25a,H25b),
 C27'(H27a,H27b), C36(H36a,H36b), C38(H38a,H38b), C34(H34a,H34b), C27(H27c,H27d)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C23(H23), C20(H20), C21(H21), C16(H16), C15(H15), C14(H14),
 C22(H22), C8(H8), C11(H11), C9(H9), C10(H10)
6.c Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C30(H30a,H30b,H30c), C28'(H28a,H28b,H28c), C37(H37a,H37b,
 H37c), C39(H39a,H39b,H39c), C35(H35a,H35b,H35c), C28(H28d,H28e,H28f)
;
_shelx_res_checksum              78238
_shelx_fab_checksum              38100
_olex2_submission_special_instructions 'No special instructions were received'