Reactivity of a Distannylene toward Potassium Graphite: Synthesis of a Stannylidenide Anion
Chia, Siew-Peng; Ganguly, Rakesh; Li, Yongxin; So, Cheuk-Wai; Organometallics 31 (2012) 6415–; doi:10.1021/om300646d

data_4079287
_publ_section_title
;
 Reactivity of a Distannylene toward Potassium Graphite: Synthesis of a
 Stannylidenide Anion
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6415
_journal_paper_doi               10.1021/om300646d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C20 H31 K N2 O Sn'
_chemical_formula_weight         473.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2822(5)
_cell_length_b                   11.0911(5)
_cell_length_c                   20.2384(12)
_cell_measurement_reflns_used    4000
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      29.75
_cell_measurement_theta_min      2.72
_cell_volume                     2308.0(2)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25101
_diffrn_reflns_theta_full        37.02
_diffrn_reflns_theta_max         37.02
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.7815
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.310
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         11182
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                8006
_reflns_number_total             11182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300646d_si_001.cif
_cod_data_source_block           scw635
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4079287