Characterization of Azulenylphosphine Derivatives. Unexpected Debromination and Its Synthetic Utility in the Preparation of 2-Substituted Azulene
Mustafizur Rahman, A. F. M.; Murafuji, Toshihiro; Shibasaki, Toshihisa; Suetake, Kouichi; Kurotobi, Kei; Sugihara, Yoshikazu; Azuma, Nagao; Mikata, Yuji; Organometallics 26 (2007) 2971–; doi:10.1021/om0607090

data_4083662
_publ_section_title
;
 Characterization of Azulenylphosphine Derivatives. Unexpected
 Debromination and Its Synthetic Utility in the Preparation of
 2-Substituted Azulene
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2971
_journal_paper_doi               10.1021/om0607090
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C22 H16 Br O P '
_chemical_formula_sum            'C22 H16 Br O P'
_chemical_formula_weight         407.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.740(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.984(5)
_cell_length_b                   9.519(5)
_cell_length_c                   18.881(10)
_cell_measurement_reflns_used    3018
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      2.1
_cell_volume                     1785.4(16)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.9904
_diffrn_measured_fraction_theta_max 0.9816
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       omega
_diffrn_radiation_type           'Mo Kalpha'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15194
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.70
_exptl_absorpt_coefficient_mu    2.405
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             824.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4072
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[sigma^2^(Fo^2^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                1765
_reflns_number_total             4546
_reflns_threshold_expression     F^2^>2.0sigma(F^2^)
_cod_data_source_file            om0607090-file003.cif
_cod_data_source_block           '__AzureneCT-050520_Compound_9'
_cod_original_cell_volume        1785.5(16)
_cod_original_formula_sum        'C22 H16 Br O P '
_cod_database_code               4083662