Pd(0)-Catalyzed Carbene Insertion into Si-Si and Sn-Sn Bonds.
Liu, Zhenxing; Tan, Haocheng; Fu, Tianren; Xia, Ying; Qiu, Di; Zhang, Yan; Wang, Jianbo; Journal of the American Chemical Society 137 (2015) 12800–12803; doi:10.1021/jacs.5b09135

data_4129644
_publ_section_title
;
 Pd(0)-Catalyzed Carbene Insertion into Si-Si and Sn-Sn Bonds.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12800
_journal_page_last               12803
_journal_paper_doi               10.1021/jacs.5b09135
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C17 H27 N O2 Sn2'
_chemical_formula_sum            'C17 H27 N O2 Sn2'
_chemical_formula_weight         514.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-06-20
_audit_creation_method
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Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4998)
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_cell_angle_alpha                90.916(2)
_cell_angle_beta                 102.405(2)
_cell_angle_gamma                91.048(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0323(2)
_cell_length_b                   10.4276(3)
_cell_length_c                   12.6489(3)
_cell_measurement_reflns_used    10741
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      29.1930
_cell_measurement_theta_min      3.8050
_cell_volume                     1034.32(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -16.00   87.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017   38.0000  120.0000 103

  2 omega   -6.00   60.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017 -112.0000  143.5345 66

  3 omega  -15.00   87.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017   38.0000    0.0000 102

  4 omega  -17.00   53.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -99.0000   60.0000 70

  5 omega  -39.00   40.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -57.0000  -60.0000 79

  6 omega  -17.00   89.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017   77.0000 -150.0000 106

  7 omega  -40.00   39.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954   57.0000 -150.0000 79
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0223320000
_diffrn_orient_matrix_UB_12      0.0156905000
_diffrn_orient_matrix_UB_13      -0.0555410000
_diffrn_orient_matrix_UB_21      -0.0380908000
_diffrn_orient_matrix_UB_22      0.0570048000
_diffrn_orient_matrix_UB_23      0.0136984000
_diffrn_orient_matrix_UB_31      0.0789286000
_diffrn_orient_matrix_UB_32      0.0336849000
_diffrn_orient_matrix_UB_33      0.0050557000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13756
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.216
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description
;
;
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.7473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3746
_reflns_number_total             4070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09135_si_002.cif
_cod_data_source_block           exp_5432
_cod_original_cell_volume        1034.31(5)
_cod_database_code               4129644
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C17 H27 O2 N1 Sn2'
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.794
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C10(H10a,H10b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.d Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C15(H15a,H15b,
 H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c)
;
_olex2_submission_special_instructions 'No special instructions were received'