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_7048017
_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 N7 Sn, 2(C F3 O3 S)'
_chemical_formula_sum            'C32 H33 F6 N7 O6 S2 Sn'
_chemical_formula_weight         908.46
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.133(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.9160(9)
_cell_length_b                   18.9906(7)
_cell_length_c                   18.5755(7)
_cell_measurement_reflns_used    9047
_cell_measurement_temperature    170
_cell_measurement_theta_max      78.251
_cell_measurement_theta_min      3.395
_cell_volume                     7601.6(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       Bruker
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      169.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            71991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.063
_diffrn_reflns_theta_min         3.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.100
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.4251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1329 before and 0.0935 after correction. The Ratio of minimum to maximum transmission is 0.5636. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       prism
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.961
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7204
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0696
_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^)+144.1608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6049
_reflns_number_total             7204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03908a2.cif
_cod_data_source_block           asrs12123_c2c_new_1
_cod_depositor_comments
'Adding full bibliography for 7048015--7048019.cif.'
_cod_database_code               7048017
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.416
_shelx_estimated_absorpt_t_min   0.203
_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
 F00I-C01I \\sim F00J-C01I
 with sigma of 0.02
 F01D-C01I \\sim F0AA-C01I
 with sigma of 0.02
 F01E-C01I \\sim F01F-C01I
 with sigma of 0.02
3. Others
 Sof(F0AA)=Sof(F01F)=Sof(F00J)=1-FVAR(1)
 Sof(F00I)=Sof(F01D)=Sof(F01E)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C00P(H00A,H00B), C00Q(H00C,H00D), C00R(H00E,H00F), C00S(H00G,H00H), C013(H01A,
 H01B), C015(H01C,H01D)
4.b Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012),
 C014(H014), C016(H016), C017(H017), C019(H019), C01A(H01H), C01G(H01L)
4.c Idealised Me refined as rotating group:
 C018(H01E,H01F,H01G), C01B(H01I,H01J,H01K), C01H(H01M,H01N,H01O)
;
_shelx_res_checksum              75659
_olex2_submission_special_instructions 'No special instructions were received'