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_7712219
_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         'C85 H78 F9 O9 P6 Pb2 S3, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C88 H81 F12 N O12 P6 Pb2 S4'
_chemical_formula_weight         2300.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-04
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.7298(2)
_cell_length_b                   29.4124(2)
_cell_length_c                   29.6444(2)
_cell_measurement_reflns_used    108232
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.6650
_cell_measurement_theta_min      2.0920
_cell_volume                     18074.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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 1.000
_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     -3.00  23.00   1.00    8.65    --    5.00  57.00  60.00   26
  2  \w    -81.00 -55.00   1.00    8.65    --   -9.00 -38.00-150.00   26
  3  \w    -39.00   4.00   1.00    8.65    --   -9.00 -38.00-150.00   43
  4  \w    -84.00  11.00   1.00    8.65    --   -9.00 -60.00  30.00   95
  5  \w    -95.00  11.00   1.00    8.65    --   -9.00 -60.00-180.00  106
  6  \w    -31.00  42.00   1.00    8.65    --   -9.00  57.00   0.00   73
  7  \w    -19.00  35.00   1.00    8.65    --   -9.00  38.00 150.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ diffractometer with Arc)Sec VHF Varimax confocal mirrors, a UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, Arc)Sec VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            274211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.689
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    4.005
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (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    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             9104
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1157
_refine_ls_number_reflns         23338
_refine_ls_number_restraints     603
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+15.7123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20986
_reflns_number_total             23338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03687h3.cif
_cod_data_source_block           '[(Pb(MeC(CH2PPh2)3))2(OTf)3][OTf]]'
_cod_depositor_comments
'Adding full bibliography for 7712208--7712219.cif.'
_cod_database_code               7712219
_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. Restrained distances
 C84-F7
 1.29 with sigma of 0.02
 C84-F8
 1.36 with sigma of 0.02
 C84-F9
 1.27 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.03
 C84-F7 \\sim C84-F8 \\sim C84-F9
 with sigma of 0.02
 C84-F9 \\sim C84-F9A
 with sigma of 0.02
 C84-F8 \\sim C84-F8A
 with sigma of 0.02
 C84-F7 \\sim C84-F7A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F9A \\sim F9 \\sim F8A \\sim F8 \\sim C84 \\sim F7A \\sim F7: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
4. Rigid body (RIGU) restrains
 Pb2, P6, P4, P5, O4, O7, C71, C70, C77, C44, C45, C51, C58, C57, C64, S2, S3,
 C76, C72, H70A, H70B, C43, C78, C82, H44A, H44B, C50, C46, C52, C56, C63, C59,
 H57A, H57B, C65, C69, O5, O6, C85, O8, O9, C84, H76, C75, H72, C73, C42, H78,
 C79, H82, C81, H50, C49, H46, C47, H52, C53, H56, C55, H63, C62, C60, H59, H65,
  C66, H69, C68, F6, F4, F5, F7, F8, F9, F7A, F8A, F9A, H75, C74, H73, H42A,
 H42B, H42C, H79, C80, H49, C48, H47, H53, C54, H55, H62, C61, H60, C67, H66,
 H68, H74, H80, H48, H54, H61, H67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C70(H70A,H70B), C16(H16A,H16B), C29(H29A,H29B), C57(H57A,
 H57B), C3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C76(H76), C50(H50), C52(H52), C49(H49), C56(H56), C46(H46), C26(H26),
 C35(H35), C11(H11), C40(H40), C78(H78), C18(H18), C63(H63), C39(H39), C27(H27),
  C61(H61), C41(H41), C15(H15), C5(H5), C82(H82), C24(H24), C60(H60), C59(H59),
 C20(H20), C13(H13), C19(H19), C79(H79), C33(H33), C47(H47), C48(H48), C9(H9),
 C12(H12), C28(H28), C55(H55), C53(H53), C34(H34), C72(H72), C14(H14), C62(H62),
  C80(H80), C65(H65), C69(H69), C54(H54), C8(H8), C75(H75), C38(H38), C31(H31),
 C32(H32), C22(H22), C25(H25), C81(H81), C74(H74), C73(H73), C37(H37), C68(H68),
  C7(H7), C21(H21), C67(H67), C6(H6), C66(H66)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C42(H42A,H42B,H42C), C88(H88A,H88B,H88C)
;
_shelx_res_checksum              16542
_shelx_hkl_checksum              19569
_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
;