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_7712211
_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         'C36 H48 F18 O18 P6 S6 Sn3, 5[C4H10O]'
_chemical_formula_sum            'C56 H98 F18 O23 P6 S6 Sn3'
_chemical_formula_weight         2215.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2539(3)
_cell_length_b                   24.0871(5)
_cell_length_c                   20.0157(5)
_cell_measurement_reflns_used    16993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8170
_cell_measurement_theta_min      1.6330
_cell_volume                     7836.3(3)
_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 0.997
_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    -21.00  64.00   0.50   25.00    --  -18.50  42.00 -48.00  170
  2  \w    -66.00   1.00   0.50   25.00    --  -18.50 107.00 170.00  134
  3  \w     22.00  64.00   0.50   25.00    --  -18.50  19.00-150.00   84
  4  \w     22.00  64.00   0.50   25.00    --  -18.50  19.00-120.00   84
  5  \w    -18.00  54.00   0.50   25.00    --   21.15 -77.00  90.00  144
  6  \w      0.00  65.00   0.50   25.00    --   21.15 -99.00 150.00  130
  7  \w     -6.00  19.00   0.50   25.00    --   21.15  57.00  30.00   50
  8  \w     -6.00  62.00   0.50   25.00    --   21.15  57.00 -90.00  136
;
_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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221645000
_diffrn_orient_matrix_UB_12      -0.0088831000
_diffrn_orient_matrix_UB_13      -0.0286054000
_diffrn_orient_matrix_UB_21      0.0360162000
_diffrn_orient_matrix_UB_22      -0.0129497000
_diffrn_orient_matrix_UB_23      -0.0125362000
_diffrn_orient_matrix_UB_31      -0.0108033000
_diffrn_orient_matrix_UB_32      -0.0249310000
_diffrn_orient_matrix_UB_33      0.0166855000
_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  0.0774
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74108
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.698
_diffrn_reflns_theta_min         2.506
_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    1.346
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84467
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         10118
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0772P)^2^+22.5651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6761
_reflns_number_total             10118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03687h3.cif
_cod_data_source_block           '[Sn(OTf)2(o-C6H4(PMe2)2)]'
_cod_depositor_comments
'Adding full bibliography for 7712208--7712219.cif.'
_cod_database_code               7712211
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SnS2F6O6P2C10H14
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.888
_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. Uiso/Uaniso restraints and constraints
C15 \\sim C15 \\sim C16 \\sim C16 \\sim H16 \\sim H16 \\sim C17 \\sim C17 \\sim
C18 \\sim C18 \\sim C19 \\sim C19 \\sim C20 \\sim C20: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, F8, C21, F9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O5A)=Sof(O6A)=Sof(C12A)=1-FVAR(1)
 Sof(S2)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(O5)=Sof(O6)=Sof(C12)=FVAR(1)
 Fixed Sof: C15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5)
 C19(0.5) H19(0.5) C20(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18), C19(H19)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 784 electrons were 
found in a volume of 1614\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5[C4H10O] per Asymmetric Unit 
which account for 840 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80898
_shelx_hkl_checksum              60565
_shelx_fab_checksum              4016
_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 2.206
_oxdiff_exptl_absorpt_empirical_full_min 0.713