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_4107059
_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            'C68 H86 N4 P4 Sn2'
_chemical_formula_weight         1320.67
_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                 104.48(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.644(2)
_cell_length_b                   17.463(2)
_cell_length_c                   26.602(2)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      1.188
_cell_volume                     6586.8(14)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            86017
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.007
_refine_diff_density_max         2.311
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         12981
_refine_ls_number_restraints     512
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0379P)^2^+9.9639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                10075
_reflns_number_total             12981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207538g_si_003.cif
_cod_data_source_block           p21c
_cod_original_cell_volume        6586.8(13)
_cod_database_code               4107059