Synthesis of Substituted Azulenes via Pt(II)-Catalyzed Ring-Expanding Cycloisomerization.
Usui, Kazuteru; Tanoue, Kensuke; Yamamoto, Kosuke; Shimizu, Takashi; Suemune, Hiroshi; Organic letters 16 (2014) 4662–; doi:10.1021/ol502270q

data_1517448
_publ_section_title
;
 Synthesis of Substituted Azulenes via Pt(II)-Catalyzed Ring-Expanding
 Cycloisomerization.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4662
_journal_paper_doi               10.1021/ol502270q
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C16 H18 O'
_chemical_formula_sum            'C16 H18 O'
_chemical_formula_weight         226.32
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_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.0000
_cell_angle_beta                 90.674(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   5.4204(7)
_cell_length_b                   12.4685(15)
_cell_length_c                   17.572(2)
_cell_measurement_temperature    90
_cell_volume                     1187.5(2)
_computing_cell_refinement       Unknown
_computing_data_collection       Unknown
_computing_data_reduction        Unknown
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Unknown CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.200
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2565
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.3822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                2257
_reflns_number_total             2565
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol502270q_si_002.cif
_cod_data_source_block           140729yamamoto_0m1
_cod_depositor_comments          'Adding full bibliography for 1517448.cif.'
_cod_original_cell_volume        1187.5(3)
_cod_database_code               1517448