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_7701862
_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         'C18 H45 Cl2 P3 Sn, 2(Al Cl4)'
_chemical_formula_sum            'C18 H45 Al2 Cl10 P3 Sn'
_chemical_formula_weight         881.60
_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             2019-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-01 deposited with the CCDC.	2019-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.560(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9000(3)
_cell_length_b                   25.4564(3)
_cell_length_c                   20.3339(4)
_cell_measurement_reflns_used    21791
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.0540
_cell_measurement_theta_min      3.1370
_cell_volume                     7605.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_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    -59.00  66.00   1.00   40.00    --  -22.90  60.00 150.00  125
  2  \w   -112.00  12.00   1.00   40.00    --  -22.90 -57.00 120.00  124
  3  \w    -58.00  66.00   1.00   40.00    --  -22.90  57.00 -90.00  124
  4  \w   -112.00 -31.00   1.00   40.00    --  -22.90 -60.00   0.00   81
  5  \w   -112.00  10.00   1.00   40.00    --  -22.90 -38.00-150.00  122
;
_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      -0.0057202000
_diffrn_orient_matrix_UB_12      -0.0249473000
_diffrn_orient_matrix_UB_13      -0.0156839000
_diffrn_orient_matrix_UB_21      0.0321171000
_diffrn_orient_matrix_UB_22      0.0069396000
_diffrn_orient_matrix_UB_23      -0.0206305000
_diffrn_orient_matrix_UB_31      0.0355940000
_diffrn_orient_matrix_UB_32      -0.0102847000
_diffrn_orient_matrix_UB_33      0.0240727000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83974
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.872
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.540
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.869
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         14932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0672P)^2^+15.0969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10136
_reflns_number_total             14932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03683k2.cif
_cod_data_source_block           sncl2pet33alcl42
_cod_database_code               7701862
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Sn Cl10 P2 C12 H30 Al2'
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.823
_reflns_odcompleteness_completeness 99.86
_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:
 C32(H32A,H32B), C16(H16A,H16B), C24(H24A,H24B), C20(H20A,H20B), C14(H14A,
 H14B), C30(H30A,H30B), C3(H3A,H3B), C28(H28A,H28B), C26(H26A,H26B), C4(H4A,
 H4B), C10(H10A,H10B), C18(H18A,H18B), C6(H6A,H6B), C34(H34A,H34B), C12(H12A,
 H12B), C8(H8A,H8B), C22(H22A,H22B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C23(H23A,H23B,
 H23C), C9(H9A,H9B,H9C), C25(H25A,H25B,H25C), C01L(H01A,H01B,H01C), C17(H17A,
 H17B,H17C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C), C13(H13A,H13B,H13C),
 C29(H29A,H29B,H29C), C5(H5A,H5B,H5C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C),
  C33(H33A,H33B,H33C), C7(H7A,H7B,H7C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              639
_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 1.758
_oxdiff_exptl_absorpt_empirical_full_min 0.480