Iron-catalyzed [2 + 2 + 2] cycloaddition of trifluoromethyl group substituted unsymmetrical internal alkynes
Minakawa, Maki; Ishikawa, Tomoki; Namioka, Junya; Hirooka, Souichirou; Zhou, Biao; Kawatsura, Motoi; RSC Adv. 4 (2014) 41353–; doi:10.1039/C4RA06973K

data_7217901
_publ_section_title
;
 Iron-catalyzed [2 + 2 + 2] cycloaddition of trifluoromethyl group
 substituted unsymmetrical internal alkynes
;
_journal_issue                   78
_journal_name_full               'RSC Adv.'
_journal_page_first              41353
_journal_paper_doi               10.1039/C4RA06973K
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C27 H23 F3 O4'
_chemical_formula_sum            'C27 H23 F3 O4'
_chemical_formula_weight         468.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                100.6126(15)
_cell_angle_beta                 103.125(6)
_cell_angle_gamma                117.338(5)
_cell_formula_units_Z            2
_cell_length_a                   9.904(4)
_cell_length_b                   10.633(4)
_cell_length_c                   13.243(5)
_cell_measurement_reflns_used    5016
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      4.69
_cell_volume                     1137.4(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      193
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0620
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23988
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5137
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0875P)^2^+0.2081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                4201
_reflns_number_total             5137
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4ra06973k2.cif
_cod_data_source_block           140310-200K-1
_cod_original_cell_volume        1137.5(7)
_cod_database_code               7217901