NHC to aNHC rearrangement by an organotin sulphide cation
Michael Wagner; Thomas Zoller; Wolf Hiller; Marc H. Prosenc; Klaus Jurkschat; Chem.Commun. 49 (2013) 8925–; doi:10.1039/c3cc45687k

data_7109814
_publ_section_title
;
 NHC to aNHC rearrangement by an organotin sulphide cation
;
_journal_name_full               Chem.Commun.
_journal_page_first              8925
_journal_paper_doi               10.1039/c3cc45687k
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C66 H118 N4 O12 P4 S2 Sn2, 2(C24 H20 B), 2(C2 H3 N)'
_chemical_formula_sum            'C118 H164 B2 N6 O12 P4 S2 Sn2'
_chemical_formula_weight         2305.55
_chemical_melting_point          444
_chemical_name_systematic
; 
{[2,6-Bis(diisopropoxyphosphonyl)-4-tert-butyl]phenyl}-tin-
[1,3-bis(tert-butyl)imidazol-4-ylidene] sulfide 
diacetonitrile solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.224(3)
_cell_angle_beta                 109.497(3)
_cell_angle_gamma                113.712(4)
_cell_formula_units_Z            1
_cell_length_a                   14.6717(5)
_cell_length_b                   14.8353(6)
_cell_length_c                   16.5591(6)
_cell_measurement_reflns_used    15533
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.6000
_cell_measurement_theta_min      2.5110
_cell_volume                     2985.3(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24''
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24''
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24''
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'enCIFer Version 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XcaliburS CCD Diffractometer'
_diffrn_measurement_method       '\w und \y scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35574
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         11099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                9808
_reflns_number_total             11099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45687k.txt
_cod_data_source_block           2408_compound1*2(CH3CN)
_cod_original_cell_volume        2985.28(19)
_cod_database_code               7109814