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_7701857
_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         'C6 H15 As Cl2 Sn0.5'
_chemical_formula_sum            'C6 H15 As Cl2 Sn0.5'
_chemical_formula_weight         292.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-27
_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                 91.301(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1388(2)
_cell_length_b                   12.1065(2)
_cell_length_c                   11.9952(3)
_cell_measurement_reflns_used    11152
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.8710
_cell_measurement_theta_min      2.3560
_cell_volume                     1036.43(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 0.914
_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   -107.00  23.00   0.50    0.92    --  -17.30 -70.00 150.00  260
  2  \w   -107.00  20.00   0.50    0.92    --  -17.30 -57.00   0.00  254
  3  \w   -107.00  23.00   0.50    0.92    --  -17.30 -70.00 -90.00  260
  4  \w    -58.00  72.00   0.50    0.92    --  -17.30  70.00 120.00  260
  5  \w   -107.00  20.00   0.50    0.92    --  -17.30 -57.00-180.00  254
  6  \w   -107.00  72.00   0.50    0.92    --  -17.30 -19.00-120.00  358
  7  \w    -58.00  22.00   0.50    0.92    --  -17.30  70.00   0.00  160
  8  \w    -58.00  72.00   0.50    0.92    --  -17.30  70.00 -60.00  260
;
_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      0.0283693000
_diffrn_orient_matrix_UB_12      0.0536342000
_diffrn_orient_matrix_UB_13      0.0172249000
_diffrn_orient_matrix_UB_21      0.0493377000
_diffrn_orient_matrix_UB_22      -0.0232164000
_diffrn_orient_matrix_UB_23      0.0463352000
_diffrn_orient_matrix_UB_31      0.0814467000
_diffrn_orient_matrix_UB_32      -0.0045960000
_diffrn_orient_matrix_UB_33      -0.0324376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27819
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.984
_diffrn_reflns_theta_min         2.391
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76463
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         3286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0195
_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^)+(0.0116P)^2^+0.7848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2799
_reflns_number_total             3286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03683k2.cif
_cod_data_source_block           vgsncl4-aset3
_cod_original_formula_sum        'C6 H15 As Cl2 Sn0.50'
_cod_database_code               7701857
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         SnCl4As2C12H30
_chemical_oxdiff_usercomment     'clear colourless'
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.792
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              61560
_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 1.733
_oxdiff_exptl_absorpt_empirical_full_min 0.719