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_7712218
_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 Ge P3, 2(C32 H12 B F24), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C105.5 H64 B2 Cl F48 Ge P3'
_chemical_formula_weight         2466.13
_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                79.1070(10)
_cell_angle_beta                 89.4620(10)
_cell_angle_gamma                69.1300(10)
_cell_formula_units_Z            2
_cell_length_a                   12.73530(10)
_cell_length_b                   16.7939(2)
_cell_length_c                   26.6298(3)
_cell_measurement_reflns_used    71142
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9110
_cell_measurement_theta_min      2.3460
_cell_volume                     5215.47(10)
_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 0.998
_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    7.50    --  -15.60 -60.00  60.00  123
  2  \w   -105.00  18.00   1.00    7.50    --  -15.60 -60.00-150.00  123
  3  \w   -105.00  18.00   1.00    7.50    --  -15.60 -60.00 -60.00  123
  4  \w    -45.00  74.00   1.00    7.50    --  -15.60  38.00-120.00  119
  5  \w    -45.00  74.00   1.00    7.50    --  -15.60  38.00-120.00  119
  6  \w   -105.00  18.00   1.00    7.50    --  -15.60 -60.00 120.00  123
  7  \w    -48.00  -1.00   1.00    7.50    --  -15.60  57.00 150.00   47
  8  \w    -49.00  74.00   1.00    7.50    --  -15.60  59.00  37.66  123
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  kat
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_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            134869
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         2.238
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90990
_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    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             2466
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1600
_refine_ls_number_reflns         26892
_refine_ls_number_restraints     1546
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+4.6793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23745
_reflns_number_total             26892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03687h3.cif
_cod_data_source_block           '[Ge(MeC(CH2PPh2)3)][BArF]2'
_cod_depositor_comments
'Adding full bibliography for 7712208--7712219.cif.'
_cod_original_formula_sum        'C105.50 H64 B2 Cl F48 Ge P3'
_cod_database_code               7712218
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.961
_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-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
 2.916 with sigma of 0.03
 Cl2-Cl1
 2.92 with sigma of 0.04
 C104-F47A \\sim C104-F3A \\sim C104-F23A \\sim C104-F3 \\sim C104-F23 \\sim
C104-F47
 with sigma of 0.02
 F47A-F3A \\sim F47A-F23A \\sim F3A-F23A \\sim F3-F23 \\sim F3-F47 \\sim F23-F47
 with sigma of 0.04
 F47-C104 \\sim F47A-C104
 with sigma of 0.02
 F3-C104 \\sim F3A-C104
 with sigma of 0.02
 F23-C104 \\sim F23A-C104
 with sigma of 0.02
 F7-C77 \\sim F7A-C77
 with sigma of 0.02
 F39-C77 \\sim F39A-C77
 with sigma of 0.02
 F7-F17 \\sim F7-F39 \\sim F17-F39 \\sim F7A-F17A \\sim F7A-F39A \\sim F17A-F39A
 with sigma of 0.04
 C77-F7 \\sim C77-F17 \\sim C77-F39 \\sim C77-F7A \\sim C77-F17A \\sim C77-F39A
 with sigma of 0.02
 F17-C77 \\sim F17A-C77
 with sigma of 0.02
 C64-F9 \\sim C64-F21 \\sim C64-F41 \\sim C64-F9A \\sim C64-F41A \\sim C64-F21A
 with sigma of 0.02
 F41-C64 \\sim F41A-C64
 with sigma of 0.02
 F21-C64 \\sim F21A-C64
 with sigma of 0.02
 F9-F21 \\sim F9-F41 \\sim F21-F41 \\sim F9A-F41A \\sim F9A-F21A \\sim F41A-F21A
 with sigma of 0.04
 F9-C64 \\sim F9A-C64
 with sigma of 0.02
 F2-C80 \\sim F2A-C80
 with sigma of 0.02
 F31-C80 \\sim F31A-C80
 with sigma of 0.02
 F5-C80 \\sim F5A-C80
 with sigma of 0.02
 C80-F2 \\sim C80-F5 \\sim C80-F31 \\sim C80-F2A \\sim C80-F5A \\sim C80-F31A
 with sigma of 0.02
 F2-F5 \\sim F2-F31 \\sim F5-F31 \\sim F2A-F5A \\sim F2A-F31A \\sim F5A-F31A
 with sigma of 0.04
 C48-F19 \\sim C48-F33 \\sim C48-F43 \\sim C48-F19A \\sim C48-F33A \\sim
C48-F43A
 with sigma of 0.02
 F19-F33 \\sim F19-F43 \\sim F33-F43 \\sim F19A-F33A \\sim F19A-F43A \\sim
F33A-F43A
 with sigma of 0.04
 F33-C48 \\sim F33A-C48
 with sigma of 0.02
 F43-C48 \\sim F43A-C48
 with sigma of 0.02
 F19-C48 \\sim F19A-C48
 with sigma of 0.02
3. Rigid bond restraints
 F9, F21, F41, C64, F9A, F41A, F21A
 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
F3 \\sim F23 \\sim F47 \\sim C104 \\sim F47A \\sim F3A \\sim F23A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F7 \\sim F17 \\sim F39 \\sim C77 \\sim F7A \\sim F17A \\sim F39A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F19 \\sim F33 \\sim F19A \\sim F43A \\sim F43 \\sim C48 \\sim F33A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F9 \\sim F21 \\sim F41 \\sim C64 \\sim F9A \\sim F41A \\sim F21A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 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
 F13, F8, C61, F16, F20, C60, C59, C62, C58, H59, H62, C63, C65, B1, C64, H65,
 C42, C50, C66, F9, F21, F41, C43, C49, C51, C57, C67, C73, H43, C44, C47, H49,
 H51, C52, C55, H57, H67, C68, C71, H73, C45, C46, C48, C53, C54, C56, C69, C70,
  C72, F25, F37, H46, F19, F33, F43, F15, F22, F27, H54, F26, F34, F40, F28,
 F38, F44, H70, F11, F45, F49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3, F23, F47, C104, F47A, F3A, F23A, C105, F2, C80, F5, F31, C79, C78, C81,
 C76, H78, H81, C74, C75, C77, B2, H75, F7, F17, F39, C82, C90, C98, C83, C89,
 C91, C97, C99, H83, C84, C87, H89, H91, C92, C95, H97, H99, C100, C103, H105,
 C85, C86, C88, C93, C94, C96, C101, C102, F29, F35, F36, H86, F10, F42, F48,
 F4, F6, F18, H94, F12, F14, F46, F24, F30, F32, H102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, F17, F39, C77, F7A, F17A, F39A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F19, F33, F43, H46, C48, F19A, F33A, F43A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F13, F25, F37, C45
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F2A, F5, F31, C80, F5A, F31A, F2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F9, F21, F41, C64, F9A, F41A, F21A
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
6. Others
 Sof(F47A)=Sof(F3A)=Sof(F23A)=1-FVAR(1)
 Sof(F3)=Sof(F23)=Sof(F47)=FVAR(1)
 Sof(F7A)=Sof(F17A)=Sof(F39A)=1-FVAR(2)
 Sof(F7)=Sof(F17)=Sof(F39)=FVAR(2)
 Sof(F9A)=Sof(F41A)=Sof(F21A)=1-FVAR(3)
 Sof(F9)=Sof(F21)=Sof(F41)=FVAR(3)
 Sof(F2A)=Sof(F5A)=Sof(F31A)=1-FVAR(4)
 Sof(F2)=Sof(F5)=Sof(F31)=FVAR(4)
 Sof(F19A)=Sof(F33A)=Sof(F43A)=1-FVAR(5)
 Sof(F19)=Sof(F33)=Sof(F43)=FVAR(5)
 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), C4(H4A,H4B), C5(H5A,H5B), C106(H10A,H10B)
7.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), 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              50152
_shelx_hkl_checksum              11805
_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
;