A regioselective double Stille coupling reaction of bicyclic stannolanes.
Kamimura, Akio; Tanaka, Toshiyuki; So, Masahiro; Itaya, Tomoyuki; Matsuda, Kantaro; Kawamoto, Takuji; Organic & biomolecular chemistry 14 (2016) 8109–8122; doi:10.1039/c6ob01018k

data_7155223
_publ_section_title
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 A regioselective double Stille coupling reaction of bicyclic stannolanes.
;
_journal_issue                   34
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8109
_journal_page_last               8122
_journal_paper_doi               10.1039/c6ob01018k
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         'C33 H48 Cl N O4 S Sn'
_chemical_formula_sum            'C33 H48 Cl N O4 S Sn'
_chemical_formula_weight         708.95
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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_block_doi                 10.5517/ccxdb1n
_audit_creation_date             2010-11-29
_audit_creation_method           'by CrystalStructure 4.0'
_audit_update_record
;
2011-09-24 deposited with the CCDC.
2016-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.4030(3)
_cell_length_b                   10.4777(4)
_cell_length_c                   36.3472(12)
_cell_measurement_reflns_used    27729
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      3.12
_cell_volume                     3581.0(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            35003
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.420
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 3550 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.023(19)
_refine_ls_extinction_coef       0.0007(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8139
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                6512
_reflns_number_total             8139
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6ob01018k2.cif
_cod_data_source_block           X-ray5
_cod_depositor_comments
;
          Adding full bibliography for 7155223.cif.

2018-02-05
Z value changed to be consistent with given formula
                 miguel
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_cod_original_formula_units_Z            5
_cod_database_code               7155223