Synthesis, spectroscopic and structural properties of Sn(II) and Pb(II) triflate complexes with soft phosphine and arsine coordination.
Cairns, Kelsey R.; King, Rhys P.; Bannister, Robert D.; Levason, William; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2293–2308; doi:10.1039/d2dt03687h

data_7712212
_publ_section_title
;
 Synthesis, spectroscopic and structural properties of Sn(II) and Pb(II)
 triflate complexes with soft phosphine and arsine coordination.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2293
_journal_page_last               2308
_journal_paper_doi               10.1039/d2dt03687h
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C36 H33 F6 O6 P3 S2 Sn, C4 H10 O'
_chemical_formula_sum            'C40 H43 F6 O7 P3 S2 Sn'
_chemical_formula_weight         1025.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-05
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-28 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.081(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8064(5)
_cell_length_b                   10.1469(2)
_cell_length_c                   27.2193(6)
_cell_measurement_reflns_used    30359
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.7300
_cell_measurement_theta_min      3.1860
_cell_volume                     4364.82(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -174.00 -90.00   0.50    1.92    -- -103.00 -45.00 -90.00  168
  2  \w   -112.00 -30.00   0.50    1.92    -- -103.00 125.00 -90.00  164
  3  \w    -70.00 -30.00   0.50    1.92    -- -103.00  61.00 -90.00   80
  4  \w   -174.00 -90.00   0.50    1.92    -- -103.00 -45.00 120.00  168
  5  \w     29.00  76.00   0.50    1.92    --  101.75 -61.00  60.00   94
  6  \w     29.00 106.00   0.50    1.92    --  101.75 -94.00  60.00  154
  7  \w     29.00  76.00   0.50    1.92    --  101.75 -61.00 -30.00   94
  8  \w     29.00  76.00   0.50    1.92    --  101.75 -61.00-150.00   94
  9  \w     29.00 125.00   0.50    1.92    --  101.75 -77.00  60.00  192
 10  \w     29.00 106.00   0.50    1.92    --  101.75 -94.00   0.00  154
 11  \w     30.00 174.00   0.50    1.92    --  101.75   0.00  30.00  288
 12  \w     89.00 175.00   0.50    1.92    --  101.75  30.00  60.00  172
 13  \w     89.00 174.00   0.50    1.92    --  101.75  45.00 -30.00  170
 14  \w     29.00 125.00   0.50    1.92    --  101.75 -77.00-150.00  192
 15  \w     29.00  76.00   0.50    1.92    --  101.75 -61.00 120.00   94
 16  \w     29.00 106.00   0.50    1.92    --  101.75 -97.00-139.18  154
 17  \w     30.00 174.00   0.50    1.92    --  101.75   0.00 150.00  288
 18  \w     82.00 175.00   0.50    1.92    --  101.75 125.00 120.00  186
 19  \w     29.00 112.00   0.50    1.92    --  101.75-125.00-120.00  166
 20  \w     29.00 106.00   0.50    1.92    --  101.75 -94.00 -60.00  154
 21  \w     29.00 106.00   0.50    1.92    --  101.75 -99.00 166.45  154
 22  \w    -16.00  29.00   0.50    0.75    --  -46.64  19.00 -90.00   90
 23  \w   -119.00 -33.00   0.50    0.75    --  -46.64 -43.00 -38.12  172
 24  \w   -118.00 -72.00   0.50    0.75    --  -46.64   0.00  60.00   92
 25  \w    -28.00  22.00   0.50    0.75    --   46.64 -19.00 -90.00  100
 26  \w    -25.00  62.00   0.50    0.75    --   46.64 -57.00  60.00  174
 27  \w     34.00 120.00   0.50    0.75    --   46.64  37.00-150.00  172
 28  \w    -25.00  62.00   0.50    0.75    --   46.64 -57.00-180.00  174
 29  \w    -28.00  22.00   0.50    0.75    --   46.64 -19.00-120.00  100
 30  \w   -119.00 -24.00   0.50    0.75    --  -46.64 -77.00  90.00  190
 31  \w   -119.00 -24.00   0.50    0.75    --  -46.64 -77.00 150.00  190
 32  \w     24.00 119.00   0.50    0.75    --   46.64  77.00 -60.00  190
 33  \w     24.00  98.00   0.50    0.75    --   46.64  77.00   0.00  148
 34  \w     24.00 119.00   0.50    0.75    --   46.64  77.00-120.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
;
Rigaku 007HF equipped with Arc)Sec VHF Varimax confocal mirrors and a UG2 goniometer and HyPix 6000HE detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_radiation_collimation    'Arc)Sec VHF Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            78496
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.198
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    7.232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.648
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         8919
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0944P)^2^+14.5010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8243
_reflns_number_total             8919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03687h3.cif
_cod_data_source_block           '[Sn(OTf)(PhP(CH2CH2PPh2)2)][OTf]'
_cod_depositor_comments
'Adding full bibliography for 7712208--7712219.cif.'
_cod_database_code               7712212
_shelx_shelxl_version_number     2018/3
_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. Rigid body (RIGU) restrains
 O7, C37, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C38(H38A,
 H38B), C39(H39A,H39B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
3.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              4215
_shelx_hkl_checksum              43604
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;