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_7712215
_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         'C44 H42 F6 O6 P4 S2 Sn, C H2 Cl2'
_chemical_formula_sum            'C45 H44 Cl2 F6 O6 P4 S2 Sn'
_chemical_formula_weight         1172.39
_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
;
2022-11-02 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1811(2)
_cell_length_b                   14.49840(10)
_cell_length_c                   21.3672(2)
_cell_measurement_reflns_used    68397
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      70.4000
_cell_measurement_theta_min      3.6510
_cell_volume                     4964.59(9)
_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      100.01(10)
_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 0.999
_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    -89.00  89.00   0.50    1.00    --    0.00  10.00 -90.00  356
  2  \w    -84.00  94.00   0.50    4.00    --    5.00  39.00   0.00  356
  3  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00-135.82  356
  4  \w   -179.00  -1.00   0.50    4.00    --  -90.00  51.00  -4.35  356
  5  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00 -65.25  356
  6  \w   -179.00  -1.00   0.50    4.00    --  -90.00  56.00 -79.43  356
  7  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00 -21.31  356
  8  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00  41.12  356
  9  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00  87.49  356
 10  \w   -179.00  -1.00   0.50    4.00    --  -90.00  58.00 116.76  356
 11  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00-174.48  356
 12  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00-174.48  356
 13  \w   -179.00  -1.00   0.50    4.00    --  -90.00  55.00-121.19  356
 14  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00   4.90  356
 15  \w   -179.00  -1.00   0.50    4.00    --  -90.00   0.00-180.00  356
 16  \w   -179.00  -1.00   0.50    4.00    --  -90.00  59.00  66.89  356
 17  \w    -89.00  89.00   0.50    1.00    --    0.00  59.00  60.00  356
 18  \w   -179.00 -55.00   0.50    4.00    --  -90.00  58.00 155.46  248
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF diffractometer 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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0230606000
_diffrn_orient_matrix_UB_12      -0.1022478000
_diffrn_orient_matrix_UB_13      0.0116769000
_diffrn_orient_matrix_UB_21      -0.0918990000
_diffrn_orient_matrix_UB_22      -0.0223803000
_diffrn_orient_matrix_UB_23      0.0052093000
_diffrn_orient_matrix_UB_31      -0.0164379000
_diffrn_orient_matrix_UB_32      -0.0183038000
_diffrn_orient_matrix_UB_33      -0.0716433000
_diffrn_radiation_collimation    'Arc)Sec VHF 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  0.0657
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            118476
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.571
_diffrn_reflns_theta_max         67.571
_diffrn_reflns_theta_min         3.696
_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    7.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53787
_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_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0688P)^2^+4.9230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8463
_reflns_number_total             8946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03687h3.cif
_cod_data_source_block           '[Sn(OTf)(P(CH2CH2PPh2)3)][OTf]'
_cod_depositor_comments
'Adding full bibliography for 7712208--7712219.cif.'
_cod_database_code               7712215
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SnS2O6F6P4C44H42
_shelx_estimated_absorpt_t_max   0.514
_shelx_estimated_absorpt_t_min   0.149
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C29(H29A,
 H29B), C30(H30A,H30B), C45(H45A,H45B)
2.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), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              75906
_shelx_hkl_checksum              51445
_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 2.956
_oxdiff_exptl_absorpt_empirical_full_min 0.627