Neutral and cationic phosphine and arsine complexes of tin(iv) halides: synthesis, properties, structures and anion influence
Greenacre, Victoria K.; King, Rhys P.; Levason, William; Reid, Gillian; Dalton Transactions  (2019) –; doi:10.1039/C9DT03683K

data_7701860
_publ_section_title
;
 Neutral and cationic phosphine and arsine complexes of tin(iv) halides:
 synthesis, properties, structures and anion influence
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03683K
_journal_year                    2019
_chemical_formula_moiety         'C13 H30 As2 Cl3 F3 O3 S Sn'
_chemical_formula_sum            'C13 H30 As2 Cl3 F3 O3 S Sn'
_chemical_formula_weight         698.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-16 deposited with the CCDC.	2019-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.21000(10)
_cell_length_b                   13.77830(10)
_cell_length_c                   13.2995(2)
_cell_measurement_reflns_used    38509
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.9270
_cell_measurement_theta_min      2.1130
_cell_volume                     2420.66(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_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    -56.00  71.00   0.50    0.50    --  -18.70  57.00  60.00  254
  2  \w    -59.00  71.00   0.50    0.50    --  -18.70  70.00 -30.00  260
  3  \w   -108.00  42.00   0.50    0.50    --  -18.70 -38.00-150.00  300
  4  \w    -59.00  71.00   0.50    0.50    --  -18.70  70.00  90.00  260
  5  \w    -59.00  71.00   0.50    0.50    --  -18.70  70.00-120.00  260
  6  \w    -59.00  71.00   0.50    0.50    --  -18.70  70.00   0.00  260
  7  \w   -108.00  22.00   0.50    0.50    --  -18.70 -70.00 150.00  260
  8  \w   -108.00 -10.00   0.50    0.50    --  -18.70 -57.00   0.00  196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0457496000
_diffrn_orient_matrix_UB_12      0.0217605000
_diffrn_orient_matrix_UB_13      -0.0164950000
_diffrn_orient_matrix_UB_21      -0.0087756000
_diffrn_orient_matrix_UB_22      0.0399114000
_diffrn_orient_matrix_UB_23      0.0325376000
_diffrn_orient_matrix_UB_31      0.0267561000
_diffrn_orient_matrix_UB_32      -0.0241194000
_diffrn_orient_matrix_UB_33      0.0388955000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66478
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.178
_diffrn_reflns_theta_min         2.128
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
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    1.916
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 3231 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         7702
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0190P)^2^+1.6885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                7415
_reflns_number_total             7702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03683k2.cif
_cod_data_source_block           sncl3(aset3)2otf
_cod_database_code               7701860
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         SnCl3As2C13H30SO3F3
_chemical_oxdiff_usercomment     'Colourless block 0.6 0.5 0.3'
_shelx_estimated_absorpt_t_max   0.364
_shelx_estimated_absorpt_t_min   0.186
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.976(6)
 0.024(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C9(H9A,H9B), C11(H11A,H11B), C1(H1A,H1B), C5(H5A,H5B), C7(H7A,H7B)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C),
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              69318
_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 1.251
_oxdiff_exptl_absorpt_empirical_full_min 0.806