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_7048019
_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         'C30 H33 F3 N7 Sn, C F3 O3 S, 4(C2 H3 N)'
_chemical_formula_sum            'C39 H45 F6 N11 O3 S Sn'
_chemical_formula_weight         980.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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
;
2018-09-25 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1425(11)
_cell_length_b                   14.5319(7)
_cell_length_c                   24.5279(12)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    170
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.93
_cell_volume                     8605.3(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0930
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            116649
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.924
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0747 before and 0.0681 after correction. The Ratio of minimum to maximum transmission is 0.9521. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       prism
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.801
_refine_diff_density_min         -2.262
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7990
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0602
_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/[\s^2^(Fo^2^)+(0.0001P)^2^+106.0581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5470
_reflns_number_total             7990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03908a2.cif
_cod_data_source_block           asrs11058_pbca
_cod_depositor_comments
'Adding full bibliography for 7048015--7048019.cif.'
_cod_database_code               7048019
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.846
_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
 N11-C37 \\sim N11'-C37'
 with sigma of 0.02
 C37-C36 \\sim C37'-C36'
 with sigma of 0.02
 N11-C36 \\sim N11'-C36'
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(N11') = Uiso(N11)
Uanis(C37') = Uanis(C37)
Uanis(C36') = Uanis(C36)
4. Others
 Fixed Sof: N11(0.5) C37(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) N11'(0.5)
 C37'(0.5) C36'(0.5) H36D(0.5) H36E(0.5) H36F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C5(H5A,H5B), C26(H26A,H26B), C28(H28A,H28B),
 C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C19(H19), C20(H20), C13(H13), C22(H22), C21(H21), C8(H8), C14(H14),
 C15(H15), C10(H10), C9(H9), C16(H16)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C27(H27A,H27B,
 H27C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C36(H36A,H36B,H36C),
 C36'(H36D,H36E,H36F)
;
_shelx_res_checksum              37712
_olex2_submission_special_instructions 'No special instructions were received'