Cationic Stannylenes: In Situ Generation and NMR Spectroscopic Characterization.
Sindlinger, Christian P.; Aicher, Frederik S. W.; Wesemann, Lars; Inorganic chemistry 56 (2017) 548–560; doi:10.1021/acs.inorgchem.6b02377

data_4345095
_publ_section_title
;
 Cationic Stannylenes: In Situ Generation and NMR Spectroscopic
 Characterization.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              548
_journal_page_last               560
_journal_paper_doi               10.1021/acs.inorgchem.6b02377
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C70 H90 N4 O2 Sn2'
_chemical_formula_weight         1256.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                105.5860(10)
_cell_angle_beta                 100.3850(10)
_cell_angle_gamma                91.9770(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2163(4)
_cell_length_b                   13.4410(4)
_cell_length_c                   18.2765(5)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      2.37
_cell_volume                     3064.22(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            71061
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.837
_diffrn_reflns_theta_min         1.686
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6323
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       prism
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         12810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+9.8563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10723
_reflns_number_total             12810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02377_si_003.cif
_cod_data_source_block           CS12b_0m
_cod_database_code               4345095
_shelxl_version_number           2014-3
_shelx_res_checksum              86816
_shelx_hkl_checksum              5869