Transition Metal-Mediated Intramolecular [2+2+2] Cycloadditions of Cyclic Triynes and Enediynes
González, Ivan; Pla-Quintana, Anna; Roglans, Anna; Torrent, Anna; Moreno-Mañas, Marcial; Parella, Teodor; Benet-Buchholz, Jordi; Journal of Organic Chemistry 70 (2005) 2033–2041; doi:10.1021/jo048056p

data_4020149
_publ_section_title
;
 Transition Metal-Mediated Intramolecular [2+2+2] Cycloadditions of
 Cyclic Triynes and Enediynes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2033
_journal_page_last               2041
_journal_paper_doi               10.1021/jo048056p
_journal_volume                  70
_journal_year                    2005
_chemical_formula_sum            'C38.5 H35 Cl2.77 Fe N3 O6 S3'
_chemical_formula_weight         886.01
_chemical_name_systematic
;
 2-Ferrocenylsulfonyl-8-[(4-methylphenyl)sulfonyl]-5-
 [(4-vinylphenyl)sulfonyl]-2,5,8-triazatrindane
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.8360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3227(4)
_cell_length_b                   11.6876(3)
_cell_length_c                   26.1060(8)
_cell_measurement_temperature    153(2)
_cell_volume                     4260.9(2)
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            'Smart 1000 CCD area detector'
_diffrn_measurement_device_type  'four-circle diffractometer Bruker P4'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans,
 in omega at 0.3 deg scan width, three runs with 98, 67 and 67 frames, phi=0 deg
 in phi at 0.3 deg scan width, two runs with 1207 frames, omega=-32 deg
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            49716
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.46
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           240
_diffrn_source_power             45
_diffrn_source_size              '10 mm x 0.5 mm fine focus'
_diffrn_source_type              'MACScience Co. M18X-HF'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.599661
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Siemens SADABS program multi-scan
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1825
_exptl_crystal_preparation
;
 Slow difusion of n-hexane into a saturated solvent mixture ethyl
 acetate/dichloromethane of the compound at room temperature
;
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         9766
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+7.1563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.2040
_reflns_number_gt                6100
_reflns_number_total             9766
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C38.50 H35 Cl2.77 Fe N3 O6 S3'
_cod_database_code               4020149