Preparation of RSn(I)-Sn(I)R with Two Unsymmetrically Coordinated Sn(I) Atoms and Subsequent Gentle Activation of P4
Shabana Khan; Reent Michel; Johannes M. Dieterich; Ricardo A. Mata; Herbert W. Roesky; Jean-Philippe Demers; Adam Lange; Dietmar Stalke; Journal of the American Chemical Society 133 (2011) 17889–17894; doi:10.1021/ja207538g

data_4107058
_publ_section_title
;
 Preparation of RSn(I)-Sn(I)R with Two Unsymmetrically Coordinated Sn(I)
 Atoms and Subsequent Gentle Activation of P4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17889
_journal_page_last               17894
_journal_paper_doi               10.1021/ja207538g
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C73 H98 N4 Sn2'
_chemical_formula_weight         1268.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 94.40(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.411(6)
_cell_length_b                   16.426(6)
_cell_length_c                   25.192(9)
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.84
_cell_measurement_theta_min      2.325
_cell_volume                     6771(4)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'INCOATEC Mo Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            177456
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         16126
_refine_ls_number_restraints     361
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+4.9847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                13617
_reflns_number_total             16126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207538g_si_002.cif
_cod_data_source_block           p21c
_cod_database_code               4107058