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_7705570
_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         'C12 F24 O4 Sn, 2(C20 H40 K O10), 2(C4 H8 O)'
_chemical_formula_sum            'C60 H96 F24 K2 O26 Sn'
_chemical_formula_weight         1886.25
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-26
_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                 114.007(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5254(11)
_cell_length_b                   10.7470(4)
_cell_length_c                   28.7368(15)
_cell_measurement_reflns_used    3755
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.597
_cell_measurement_theta_min      2.373
_cell_volume                     7765.4(6)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_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_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24929
_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         26.418
_diffrn_reflns_theta_min         1.620
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0524 before and 0.0486 after correction. The Ratio of minimum to maximum transmission is 0.9324. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         7963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0246P)^2^+4.8090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6116
_reflns_number_total             7963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02837a2.cif
_cod_data_source_block           lhd568_0m_a_Compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7705569--7705573.cif.
;
_cod_database_code               7705570
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.852
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C11(H11A,H11B), C24(H24A,H24B), C16(H16A,H16B), C25(H25A,
 H25B), C28(H28A,H28B), C22(H22A,H22B), C26(H26A,H26B), C20(H20A,H20B),
 C19(H19A,H19B), C17(H17A,H17B), C12(H12A,H12B), C18(H18A,H18B), C23(H23A,H23B),
  C21(H21A,H21B), C29(H29A,H29B), C30(H30A,H30B), C14(H14A,H14B), C15(H15A,
 H15B), C13(H13A,H13B), C9(H9A,H9B), C8(H8A,H8B), C10(H10A,H10B), C7(H7A,H7B)
;
_shelx_res_checksum              49784
_olex2_submission_special_instructions 'No special instructions were received'