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_7109815
_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), 4(C4 H8 O)'
_chemical_formula_sum            'C130 H190 B2 N4 O16 P4 S2 Sn2'
_chemical_formula_weight         2511.86
_chemical_melting_point          448
_chemical_name_systematic
; 
 {[2,6-Bis(diisopropoxyphosphonyl)-4-tert-butyl]phenyl}-tin-
[1,3-bis(tert-butyl)imidazol-4-ylidene]sulfide 
tetratetrahydrofurane 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                75.857(2)
_cell_angle_beta                 81.874(2)
_cell_angle_gamma                70.110(2)
_cell_formula_units_Z            1
_cell_length_a                   15.1046(4)
_cell_length_b                   15.2266(5)
_cell_length_c                   15.9520(4)
_cell_measurement_reflns_used    18738
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.6950
_cell_measurement_theta_min      2.5840
_cell_volume                     3338.57(17)
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39686
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97596
_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    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         12421
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                10762
_reflns_number_total             12421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45687k.txt
_cod_data_source_block           a2396p1-sr_compound1*4THF
_cod_original_cell_volume        3338.58(16)
_cod_database_code               7109815