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_4083661
_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 H15 Br2 O P '
_chemical_formula_sum            'C22 H15 Br2 O P'
_chemical_formula_weight         486.14
_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                 101.34(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.707(6)
_cell_length_b                   31.633(7)
_cell_length_c                   9.144(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10.1
_cell_volume                     1902.1(19)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  'teXsan Ver. 2.0'
_computing_structure_solution    SHELXS97
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9993
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4822
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_decay_%        0.64
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.367
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             960.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.14
_refine_diff_density_min         -1.61
_refine_ls_extinction_coef       0.017(2)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4365
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.10000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1964
_reflns_number_gt                2292
_reflns_number_total             4720
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om0607090-file003.cif
_cod_data_source_block           '[azulene-PO-ph2_Compound_3b]'
_cod_original_cell_volume        1902(1)
_cod_original_sg_symbol_H-M      'P 21/n       '
_cod_original_formula_sum        'C22 H15 Br2 O P '
_cod_database_code               4083661