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_7701861
_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         'C12 H30 As2 Br4 Sn'
_chemical_formula_sum            'C12 H30 As2 Br4 Sn'
_chemical_formula_weight         762.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-23
_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                   13.8250(2)
_cell_length_b                   11.0254(2)
_cell_length_c                   14.4329(2)
_cell_measurement_reflns_used    24616
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.4710
_cell_measurement_theta_min      2.7180
_cell_volume                     2199.95(6)
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55967
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.026
_diffrn_reflns_theta_min         2.752
_exptl_absorpt_coefficient_mu    11.401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65876
_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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.302
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.423
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         3615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0358
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3286
_reflns_number_total             3615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03683k2.cif
_cod_data_source_block           ov_vgsnbr4aset3
_cod_database_code               7701861
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.342
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4A(0.026) H4B(0.026) H4C(0.026) H1A(0.02) H1B(0.02) H5A(0.02)
 H5B(0.02) H3A(0.019) H3B(0.019) H6A(0.033) H6B(0.033) H6C(0.033) H2A(0.031)
 H2B(0.031) H2C(0.031)
 Fixed X: Sn1(0.5) H4A(0.668222) H4B(0.681517) H4C(0.622942) H1A(0.466409)
 H1B(0.353726) H5A(0.299552) H5B(0.286268) H3A(0.516386) H3B(0.559541)
 H6A(0.39017) H6B(0.293368) H6C(0.392884) H2A(0.382499) H2B(0.466532)
 H2C(0.356276)
 Fixed Y: Sn1(0.5) H4A(0.721209) H4B(0.814124) H4C(0.85454) H1A(0.843)
 H1B(0.815149) H5A(0.738264) H5B(0.60961) H3A(0.805135) H3B(0.670693)
 H6A(0.521094) H6B(0.575873) H6C(0.649309) H2A(1.013632) H2B(0.968724)
 H2C(0.934524)
 Fixed Z: Sn1(0.5) H4A(0.614398) H4B(0.698627) H4C(0.60811) H1A(0.481791)
 H1B(0.495216) H5A(0.690506) H5B(0.640781) H3A(0.732445) H3B(0.733841)
 H6A(0.756156) H6B(0.800266) H6C(0.808067) H2A(0.545435) H2B(0.613542)
 H2C(0.634943)
;
_shelx_res_checksum              29473
_olex2_submission_special_instructions 'No special instructions were received'