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_7705573
_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         'C18 F36 O6 Sn, 2(C6 H16 N), 2(C3 H6 O)'
_chemical_formula_sum            'C36 H44 F36 N2 O8 Sn'
_chemical_formula_weight         1435.42
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-04-17 deposited with the CCDC.	2020-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                82.239(2)
_cell_angle_beta                 80.467(2)
_cell_angle_gamma                70.003(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3859(9)
_cell_length_b                   14.3035(11)
_cell_length_c                   15.7748(13)
_cell_measurement_reflns_used    6660
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.438
_cell_measurement_theta_min      2.331
_cell_volume                     2580.6(3)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX CCD'
_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 X8 APEX'
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34045
_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         28.320
_diffrn_reflns_theta_min         1.764
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.5193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0467 before and 0.0433 after correction. The Ratio of minimum to maximum transmission is 0.9219. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.095
_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     758
_refine_ls_number_reflns         12802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0224P)^2^+0.5754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9984
_reflns_number_total             12802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02837a2.cif
_cod_data_source_block           lhd528_0m_a_Compound_1
_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               7705573
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C28(H28A,H28B), C26(H26A,H26B), C21(H21A,H21B), C23(H23A,
 H23B), C20(H20A,H20B)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C27(H27A,H27B,H27C), C19(H19A,H19B,H19C), C22(H22A,H22B,
 H22C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C34(H34A,
 H34B,H34C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              17025
_olex2_submission_special_instructions 'No special instructions were received'