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_7712210
_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         'C12 H16 As2 F6 O6 Pb S2'
_chemical_formula_sum            'C12 H16 As2 F6 O6 Pb S2'
_chemical_formula_weight         791.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 95.1510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.58200(10)
_cell_length_b                   21.4899(2)
_cell_length_c                   9.72860(10)
_cell_measurement_reflns_used    15788
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.1580
_cell_measurement_theta_min      4.6460
_cell_volume                     2203.41(4)
_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_environment      N~2~
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -89.00  77.00   0.50    0.50    --    0.00   0.00-180.00  332
  2  \w   -112.00 -75.00   0.50    0.50    --  -90.00  57.00  99.53   74
  3  \w    -64.00 -30.00   0.50    0.50    --  -90.00  30.00-150.00   68
  4  \w    -63.00  -2.00   0.50    0.50    --  -90.00  49.00  30.00  122
  5  \w   -177.00-128.00   0.50    0.50    --  -90.00  48.00 -74.50   98
  6  \w   -179.00 -70.00   0.50    0.50    --  -90.00  30.00-150.00  218
  7  \w    -69.00  -1.00   0.50    0.50    --  -90.00  55.00-154.04  136
  8  \w   -157.00-131.00   0.50    0.50    --  -90.00  39.00-180.00   52
  9  \w   -152.00 -99.00   0.50    0.50    --  -90.00  49.00  30.00  106
 10  \w   -179.00 -92.00   0.50    0.50    --  -90.00  57.00  32.56  174
 11  \w   -177.00-152.00   0.50    0.50    --  -90.00  58.00 -37.06   50
 12  \w   -115.00 -64.00   0.50    0.50    --  -90.00  58.00 -37.06  102
 13  \w    -40.00  -5.00   0.50    0.50    --  -90.00  58.00 -37.06   70
 14  \w   -120.00 -94.00   0.50    0.50    --  -90.00  55.00-154.04   52
 15  \w   -122.00 -30.00   0.50    0.50    --  -90.00  48.00 -74.50  184
 16  \w   -179.00-124.00   0.50    0.50    --  -90.00  20.00 -60.00  110
 17  \w    -78.00 -52.00   0.50    0.50    --  -90.00  20.00 -60.00   52
 18  \w    -47.00 -22.00   0.50    0.50    --  -90.00  57.00  99.53   50
 19  \w    -49.00 -23.00   0.50    0.50    --  -90.00  39.00-180.00   52
 20  \w   -105.00 -79.00   0.50    0.50    --  -90.00  39.00  30.00   52
 21  \w    -62.00 -36.00   0.50    0.50    --  -90.00  39.00  30.00   52
 22  \w   -178.00-140.00   0.50    0.50    --  -90.00  57.00  99.53   76
 23  \w   -178.00-153.00   0.50    0.50    --  -90.00  30.00 -30.00   50
 24  \w   -148.00-122.00   0.50    0.50    --  -90.00  39.00 -30.00   52
 25  \w   -137.00 -66.00   0.50    0.50    --  -90.00  49.00-120.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF diffractometer with HF Varimax confocal mirrors, an UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1051566000
_diffrn_orient_matrix_UB_12      -0.0477449000
_diffrn_orient_matrix_UB_13      0.0415148000
_diffrn_orient_matrix_UB_21      -0.0981382000
_diffrn_orient_matrix_UB_22      -0.0425248000
_diffrn_orient_matrix_UB_23      0.0608447000
_diffrn_orient_matrix_UB_31      -0.0261776000
_diffrn_orient_matrix_UB_32      -0.0323837000
_diffrn_orient_matrix_UB_33      -0.1409141000
_diffrn_radiation_collimation    'HF Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21504
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.556
_diffrn_reflns_theta_max         67.556
_diffrn_reflns_theta_min         4.673
_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    20.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43210
_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            'light yellow'
_exptl_crystal_density_diffrn    2.386
_exptl_crystal_description       needle
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.556
_refine_diff_density_min         -2.416
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3966
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0247P)^2^+14.7498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3912
_reflns_number_total             3966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03687h3.cif
_cod_data_source_block           '[Pb(OTf)2(o-C6H4(AsMe2)2)]'
_cod_depositor_comments
'Adding full bibliography for 7712208--7712219.cif.'
_cod_database_code               7712210
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         PbAs2S2O6F6C12H16
_chemical_oxdiff_usercomment     'Pb + diars?'
_shelx_estimated_absorpt_t_max   0.424
_shelx_estimated_absorpt_t_min   0.063
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 S2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Pb1, As1, As2, S1, S2, F6, F4, F1, F2, F3, F5, O1, O2, O3, O4, O5, O6, C00R,
 C1, H1A, H1B, H1C, C2, H2A, H2B, H2C, C3, C4, H4, C5, H5, C6, H6, C7, H7, C8,
 C9, H9A, H9B, H9C, C10, H10A, H10B, H10C, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F3, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              53845
_shelx_hkl_checksum              71174
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.992
_oxdiff_exptl_absorpt_empirical_full_min 0.684