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_7048018
_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 F2 N7 Sn, 2(C F3 O3 S), 1.5(C2 H3 N)'
_chemical_formula_sum            'C35 H37.5 F8 N8.5 O6 S2 Sn'
_chemical_formula_weight         1008.04
_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
;
2018-09-25 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.894(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3989(11)
_cell_length_b                   15.9087(13)
_cell_length_c                   18.4727(14)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.86
_cell_volume                     4226.1(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0646
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            142018
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.865
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.793
_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    1.584
_exptl_crystal_description       prism
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7423
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0692
_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^)+51.3073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5607
_reflns_number_total             7423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03908a2.cif
_cod_data_source_block           asrs11058_1_p21c
_cod_depositor_comments
'Adding full bibliography for 7048015--7048019.cif.'
_cod_original_formula_sum        'C35 H37.50 F8 N8.50 O6 S2 Sn'
_cod_database_code               7048018
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.814
_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. Rigid bond restraints
 N9, C33, C34
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: C34(0.5) H34a(0.5) H34b(0.5) H34c(0.5) C33(0.5) N9(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C5(H5a,H5b), C3(H3a,H3b), C29(H29a,H29b), C25(H25a,H25b),
 C27(H27a,H27b)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C21(H21), C23(H23), C20(H20), C22(H22), C8(H8), C9(H9),
 C17(H17), C16(H16), C14(H14), C15(H15)
4.c Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C32(H32a,H32b,H32c), C30(H30a,H30b,H30c), C28(H28a,H28b,
 H28c), C34(H34a,H34b,H34c)
;
_shelx_res_checksum              6110
_olex2_submission_special_instructions 'No special instructions were received'