Alkylthio Unit as an α-Pyrrole Protecting Group for Use in Dipyrromethane Synthesis
Patchanita Thamyongkit; Anil D. Bhise; Masahiko Taniguchi; Jonathan S. Lindsey; Journal of Organic Chemistry 71 (2006) 903–910; doi:10.1021/jo051806q

data_4021426
_publ_contact_author_address
;Department of Chemistry
North Carolina State University
Raleigh, NC 27695-8204
USA
;
_publ_contact_author_email       jlindsey@ncsu.edu
_publ_contact_author_fax         919-513-2830
_publ_contact_author_name        'Jonathan S. Lindsey'
_publ_contact_author_phone       919-515-6406
_publ_section_title
;
 Alkylthio Unit as an \a-Pyrrole Protecting Group
 for Use in Dipyrromethane Synthesis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              903
_journal_page_last               910
_journal_paper_doi               10.1021/jo051806q
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C35 H38 N2 O4 S2 Sn '
_chemical_formula_sum            'C35 H38 N2 O4 S2 Sn'
_chemical_formula_weight         733.50
_chemical_name_common
;
Dibutyl[5,10-dihydro-1,9-bis(phenylsulfonyl)-5-phenyldipyrrinato]tin(IV)
;
_chemical_name_systematic
;
Dibutyl[5,10-dihydro-1,9-bis(phenylsulfonyl)-5-phenyldipyrrinato]tin(IV)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 92.2023(15)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   8.5613(2)
_cell_length_b                   15.6149(4)
_cell_length_c                   12.0541(3)
_cell_measurement_reflns_used    8604
_cell_measurement_temperature    110
_cell_measurement_theta_max      34.53
_cell_measurement_theta_min      2.71
_cell_volume                     1610.25(7)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        SAINT+
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      110
_diffrn_measurement_device       'Bruker-Nonius X8 Apex2'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .030
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            132249
_diffrn_reflns_theta_max         41.87
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    .96
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8845
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       'translucent prism'
_exptl_crystal_F_000             751.57
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .26
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.00
_refine_diff_density_min         -1.07
_refine_ls_extinction_coef       0.17(2)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_obs   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         18798
_refine_ls_R_factor_all          .039
_refine_ls_R_factor_obs          .030
_refine_ls_shift/esd_max         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '1/(\s^2^(F)+ .0002F^2^) '
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .034
_refine_ls_wR_factor_obs         .025
_reflns_number_observed          18800
_reflns_number_total             21349
_reflns_observed_criterion       'Inet > 1.0\s(Inet)'
_cod_data_source_file            jo051806qsi20050902_021349.cif
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C35 H38 N2 O4 S2 Sn '
_cod_database_code               4021426