Stannylene-Based Lewis Pairs
Freitag, Sarah; Krebs, Kilian M.; Henning, Jens; Hirdler, Janina; Schubert, Hartmut; Wesemann, Lars; Organometallics 32 (2013) 6785–; doi:10.1021/om400736e

data_4081884
_publ_section_title
;
 Stannylene-Based Lewis Pairs
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6785
_journal_paper_doi               10.1021/om400736e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C62 H69 P Sn, 0.5(C6 H6), 0.5(C5 H12)'
_chemical_formula_sum            'C65 H72 P Sn'
_chemical_formula_weight         1002.89
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0458(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4011(5)
_cell_length_b                   18.8054(8)
_cell_length_c                   24.7687(10)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.0797
_cell_measurement_theta_min      2.2647
_cell_volume                     5768.1(4)
_computing_cell_refinement       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_collection       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX--II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            182209
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.9389
_exptl_absorpt_correction_T_min  0.7999
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
The structure contains 2 molecules of pentane and/or benzene 
per unit cell in the squeezed area.
;
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         13235
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+5.5784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                12269
_reflns_number_total             13235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400736e_si_002.cif
_cod_data_source_block           SnPhPHCCPh
_cod_database_code               4081884
_computing_bruker_data_scaling   'SADABS V2008/1 (Bruker AXS)'