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_7705572
_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         '0.5(C40 H32 F48 K4 O12 Sn2)'
_chemical_formula_sum            'C20 H16 F24 K2 O6 Sn'
_chemical_formula_weight         1005.22
_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'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 95.237(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6806(14)
_cell_length_b                   12.1477(10)
_cell_length_c                   14.6638(13)
_cell_measurement_reflns_used    3839
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.44
_cell_volume                     2958.9(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0648
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11885
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.361
_diffrn_reflns_theta_min         2.077
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0793 before and 0.0746 after correction. The Ratio of minimum to maximum transmission is 0.9161. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.256
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0325P)^2^+11.8516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3119
_reflns_number_total             3676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02837a2.cif
_cod_data_source_block           lhd553_0m_a_Compound_4
_cod_depositor_comments
'Adding full bibliography for 7705569--7705573.cif.'
_cod_database_code               7705572
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2AA) = Uanis(C4AA)
Uanis(C1AA) = Uanis(C4AA)
Uanis(C3AA) = Uanis(C2AA)
3. Others
 Fixed Sof: H3AA(0.4) H3AB(0.4) H3AC(0.6) H3AD(0.6) H1AA(0.4) H1AB(0.4)
 H1AC(0.6) H1AD(0.6) C4AA(0.4) H4AA(0.4) H4AB(0.4) C2AA(0.6) H2AA(0.6) H2AB(0.6)
4.a Secondary CH2 refined with riding coordinates:
 C3AA(H3AA,H3AB), C3AA(H3AC,H3AD), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C1AA(H1AC,
 H1AD), C4AA(H4AA,H4AB), C2AA(H2AA,H2AB)
;
_shelx_res_checksum              87678
_olex2_submission_special_instructions 'No special instructions were received'