Formation of monomeric Sn(ii) and Sn(iv) perfluoropinacolate complexes and their characterization by <sup>119</sup>Sn Mössbauer and <sup>119</sup>Sn NMR spectroscopies.
Elinburg, Jessica K.; Hyre, Ariel S.; McNeely, James; Alam, Todd M.; Klenner, Steffen; Pöttgen, Rainer; Rheingold, Arnold L.; Doerrer, Linda H.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13773–13785; doi:10.1039/d0dt02837a

data_7705571
_publ_section_title
;
 Formation of monomeric Sn(ii) and Sn(iv) perfluoropinacolate complexes
 and their characterization by <sup>119</sup>Sn M\"ossbauer and
 <sup>119</sup>Sn NMR spectroscopies.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13773
_journal_page_last               13785
_journal_paper_doi               10.1039/d0dt02837a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C24 H12 F36 K O9 Sn, C15 H30 K O7'
_chemical_formula_sum            'C39 H42 F36 K2 O16 Sn'
_chemical_formula_weight         1647.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-04-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-17 deposited with the CCDC.	2020-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                99.540(3)
_cell_angle_beta                 114.932(3)
_cell_angle_gamma                112.822(3)
_cell_formula_units_Z            2
_cell_length_a                   15.1378(16)
_cell_length_b                   16.2438(16)
_cell_length_c                   16.2454(16)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.35
_cell_volume                     3068.9(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47361
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.421
_diffrn_reflns_theta_min         1.480
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0449 before and 0.0406 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1584 before and 0.0617 after correction.
 The Ratio of minimum to maximum transmission is 0.75.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 68084 reflections, Rint = 0.0495
 (34871 with I > 3sig(I), Rint = 0.0420)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.576
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         11297
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0344P)^2^+8.2804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9851
_reflns_number_total             11297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02837a2.cif
_cod_data_source_block           lhd534_a_sq_Compound_3
_cod_depositor_comments
'Adding full bibliography for 7705569--7705573.cif.'
_cod_original_cell_volume        3068.9(5)
_cod_database_code               7705571
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.813
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3AA-C0AA
 1.5 with sigma of 0.002
 C0AA-C5AA
 1.5 with sigma of 0.002
 C2AA-C1AA
 1.5 with sigma of 0.002
3. Others
 Fixed Sof: C2AA(0.6) H2AA(0.6) H2AB(0.6) H2AC(0.6) C4AA(0.4) H4AA(0.4)
 H4AB(0.4) H4AC(0.4) O0AA(0.6) O1AA(0.4) C0AA(0.6) C1AA(0.4) C3AA(0.6)
 H3AA(0.6) H3AB(0.6) H3AC(0.6) C5AA(0.4) H5AA(0.4) H5AB(0.4) H5AC(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C22(H22A,H22B), C23(H23A,H23B), C21(H21A,H21B), C25(H25A,
 H25B), C35(H35A,H35B), C26(H26A,H26B), C24(H24A,H24B), C30(H30A,H30B),
 C33(H33A,H33B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B),
  C32(H32A,H32B), C34(H34A,H34B)
4.b Me refined with riding coordinates:
 C2AA(H2AA,H2AB,H2AC), C4AA(H4AA,H4AB,H4AC), C3AA(H3AA,H3AB,H3AC), C5AA(H5AA,
 H5AB,H5AC)
;
_shelx_res_checksum              52585
_shelx_fab_checksum              83980
_olex2_submission_special_instructions 'No special instructions were received'