Absolute Configuration of 2-(Tributylstannyl)pyrrolidine by Anomalous Dispersion X-ray Analysis
Robert E. Gawley; Sanjay Narayan; David A. Vicic; Journal of Organic Chemistry 70 (2005) 328–329; doi:10.1021/jo048569w

data_4020013
_publ_section_title
;
Absolute Configuration of 2-(Tributylstannyl)pyrrolidine by Anomalous
Dispersion X-ray Analysis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              328
_journal_page_last               329
_journal_paper_doi               10.1021/jo048569w
_journal_volume                  70
_journal_year                    2005
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C32 H72 I2 N2 Sn2'
_chemical_formula_sum            'C32 H72 I2 N2 Sn2'
_chemical_formula_weight         976.12
_chemical_melting_point          ?
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 117.75(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.04(6)
_cell_length_b                   9.16(3)
_cell_length_c                   16.62(10)
_cell_measurement_reflns_used    86
_cell_measurement_temperature    193.1
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      2.4
_cell_volume                     2162.7(17)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.9919
_diffrn_measured_fraction_theta_max 0.8823
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.117
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19404
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         34.92
_exptl_absorpt_coefficient_mu    2.602
_exptl_absorpt_correction_T_max  0.594
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             968.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         6.44
_refine_diff_density_min         -6.77
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.1(1)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   14.209
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     164
_refine_ls_number_reflns         13115
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          6.8800
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1.0'
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                6008
_reflns_number_total             19404
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_database_code               4020013