Base-mediated cyclization reaction of 2-alkynylphenylphosphine oxides: synthesis and photophysical properties of benzo[b]phosphole oxides.
Sanji, Takanobu; Shiraishi, Kentaro; Kashiwabara, Taigo; Tanaka, Masato; Organic letters 10 (2008) 2689–2692; doi:10.1021/ol800841v

data_1504711
_publ_section_title
;
 Base-mediated cyclization reaction of 2-alkynylphenylphosphine oxides:
 synthesis and photophysical properties of benzo[b]phosphole oxides.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              2689
_journal_page_last               2692
_journal_paper_doi               10.1021/ol800841v
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C44 H42 Cl6 O2 P2 '
_chemical_formula_sum            'C44 H42 Cl6 O2 P2'
_chemical_formula_weight         877.48
_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'
_cell_angle_alpha                106.891(4)
_cell_angle_beta                 96.650(4)
_cell_angle_gamma                95.930(4)
_cell_formula_units_Z            2
_cell_length_a                   12.273(4)
_cell_length_b                   13.405(5)
_cell_length_c                   14.376(5)
_cell_measurement_reflns_used    6041
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2224.4(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
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_diffrn_detector_area_resol_mean 29.26
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16896
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             908.00
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.85
_refine_diff_density_min         -1.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     529
_refine_ls_number_reflns         5599
_refine_ls_R_factor_gt           0.0941
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0239Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1492
_reflns_number_gt                5599
_reflns_number_total             9535
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol800841v-file003.cif
_cod_data_source_block           '___srs080322-2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'No' changed to 'no' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (100
times).

'_geom_angle_publ_flag' value 'No' changed to 'no' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (174 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C44 H42 Cl6 O2 P2 '
_cod_database_code               1504711