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_7712217
_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
'C41 H39 P3 Pb, 2(C32 H12 B F24), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C105.5 H64 B2 Cl F48 P3 Pb'
_chemical_formula_weight         2600.73
_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
_audit_creation_date             2022-10-27
_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                78.0880(10)
_cell_angle_beta                 89.0490(10)
_cell_angle_gamma                69.7610(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7607(2)
_cell_length_b                   16.7182(2)
_cell_length_c                   26.6413(3)
_cell_measurement_reflns_used    72805
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9760
_cell_measurement_theta_min      2.2480
_cell_volume                     5208.49(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_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_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -105.00  18.00   1.00    1.37    --  -15.80 -60.00  60.00  123
  2  \w   -105.00  17.00   1.00    1.37    --  -15.80 -57.00 120.00  122
  3  \w   -105.00  18.00   1.00    1.37    --  -15.80 -60.00 -90.00  123
  4  \w   -105.00  18.00   1.00    1.37    --  -15.80 -60.00-150.00  123
  5  \w   -105.00  14.00   1.00    1.37    --  -15.80 -38.00 -90.00  119
  6  \w   -105.00  18.00   1.00    1.37    --  -15.80 -60.00  30.00  123
  7  \w    -49.00  -2.00   1.00    1.37    --  -15.80  60.00 150.00   47
  8  \w    -49.00  74.00   1.00    1.37    --  -15.80  60.00 -30.00  123
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            134409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.996
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
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    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             2566
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1544
_refine_ls_number_reflns         26898
_refine_ls_number_restraints     1392
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+5.4428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24915
_reflns_number_total             26898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03687h3.cif
_cod_data_source_block           '[Pb(MeC(CH2PPh2)3)][BArF]2'
_cod_depositor_comments
'Adding full bibliography for 7712208--7712219.cif.'
_cod_original_cell_volume        5208.49(12)
_cod_original_formula_sum        'C105.50 H64 B2 Cl F48 P3 Pb'
_cod_database_code               7712217
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.610
_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
 Cl2-Cl1
 2.916 with sigma of 0.03
 Cl2-C106
 1.78 with sigma of 0.02
 Cl1-C106
 1.77 with sigma of 0.02
 Cl2-C106 = Cl1-C106
 1.771 with sigma of 0.01
 Cl2-Cl1
 2.92 with sigma of 0.04
 C77-F45 \\sim C77-F25
 with sigma of 0.02
 C77-F47 \\sim C77-F49
 with sigma of 0.04
 F23-F47 \\sim F3-F49
 with sigma of 0.02
 C77-F23 \\sim C77-F3
 with sigma of 0.02
 C77-F45 \\sim C77-F23 \\sim C77-F47 \\sim C77-F3 \\sim C77-F49 \\sim C77-F25
 with sigma of 0.02
 F45-F23 \\sim F45-F47 \\sim F23-F47 \\sim F3-F49 \\sim F3-F25 \\sim F49-F25
 with sigma of 0.04
 F43-C48 \\sim F51-C48
 with sigma of 0.02
 F5-C48 \\sim F13-C48
 with sigma of 0.02
 F41-C48 \\sim F53-C48
 with sigma of 0.02
 F5-F41 \\sim F5-F43 \\sim F41-F43 \\sim F51-F13 \\sim F51-F53 \\sim F13-F53
 with sigma of 0.04
 C48-F5 \\sim C48-F41 \\sim C48-F43 \\sim C48-F51 \\sim C48-F13 \\sim C48-F53
 with sigma of 0.02
 F2-F19 \\sim F2-F31 \\sim F19-F31 \\sim F27-F55 \\sim F27-F7 \\sim F55-F7
 with sigma of 0.04
 F2-C80 \\sim F27-C80
 with sigma of 0.02
 C80-F2 \\sim C80-F19 \\sim C80-F31 \\sim C80-F27 \\sim C80-F55 \\sim C80-F7
 with sigma of 0.02
 F19-C80 \\sim F7-C80
 with sigma of 0.02
 F31-C80 \\sim F55-C80
 with sigma of 0.02
3. Rigid bond restraints
 C48, F5, F41, F43, F13, F51, F53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C106: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C77 \\sim F23 \\sim F45 \\sim F47 \\sim F3 \\sim F25 \\sim F49: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C80 \\sim F2 \\sim F19 \\sim F31 \\sim F7 \\sim F27 \\sim F55: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C48 \\sim F5 \\sim F41 \\sim F43 \\sim F13 \\sim F51 \\sim F53: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 Cl1, Cl2, C106
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C77, F23, F45, F47, F3, F25, F49
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C48, F5, F41, F43, F13, F51, F53
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F8, F9, F11, F14, F17, F18, F20, F21, F28, F29, F30, F32, F33, F35, F36, F39,
 F42, F44, F48, F50, F57, C42, C43, H43, C44, C45, C46, H46, C47, C48, C49, H49,
  C50, C51, H51, C52, C53, C54, H54, C55, C56, C57, H57, C58, C59, H59, C60,
 C61, C62, H62, C63, C64, C65, H65, C66, C67, H67, C68, C69, C70, H70, C71, C72,
  C73, H73, B1, F5, F41, F43, F13, F51, F53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F4, F6, F10, F12, F15, F16, F22, F24, F26, F34, F37, F38, F40, F46, F52,
 F54, F56, C74, C75, H75, C76, C77, C78, H78, C79, C80, C81, H81, C82, C83, H83,
  C84, C85, C86, H86, C87, C88, C89, H89, C90, C91, H91, C92, C93, C94, H94,
 C95, C96, C97, H97, C98, C99, H99, C100, C101, C102, H102, C103, C104, C105,
 H105, B2, F2, F19, F23, F31, F45, F47, F3, F7, F25, F27, F49, F55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C80, F2, F19, F31, F7, F27, F55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F17, F36, F57, C61
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F33, F35, F39, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F11, F21, F44, C69
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 F15, F37, F46, C85
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
6. Others
 Sof(F3)=Sof(F25)=Sof(F49)=1-FVAR(1)
 Sof(F23)=Sof(F45)=Sof(F47)=FVAR(1)
 Sof(F13)=Sof(F51)=Sof(F53)=1-FVAR(2)
 Sof(F5)=Sof(F41)=Sof(F43)=FVAR(2)
 Sof(F7)=Sof(F27)=Sof(F55)=1-FVAR(3)
 Sof(F2)=Sof(F19)=Sof(F31)=FVAR(3)
 Fixed Sof: Cl1(0.5) Cl2(0.5) C106(0.5) H10A(0.5) H10B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C16(H16A,H16B), C29(H29A,H29B), C106(H10A,H10B)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C75(H75),
  C78(H78), C81(H81), C83(H83), C86(H86), C89(H89), C91(H91), C94(H94),
 C97(H97), C99(H99), C102(H102), C105(H105), C43(H43), C46(H46), C49(H49),
 C51(H51), C54(H54), C57(H57), C59(H59), C62(H62), C65(H65), C67(H67), C70(H70),
  C73(H73)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              37348
_shelx_hkl_checksum              92937
_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
;