Dibenzo[b,e]phosphindolizines Synthesized by Ring-Closing Metathesis of Benzo[b]phospholes with Two Vinyl Tethers
Tsurusaki, Akihiro; Matsumoto, Hiroyo; Kamikawa, Ken; Chemical Communications  (2019) –; doi:10.1039/C9CC00463G

data_7123141
_publ_section_title
;
 Dibenzo[b,e]phosphindolizines Synthesized by Ring-Closing Metathesis of
 Benzo[b]phospholes with Two Vinyl Tethers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00463G
_journal_year                    2019
_chemical_formula_moiety         'C16 H11 P S'
_chemical_formula_sum            'C16 H11 P S'
_chemical_formula_weight         266.28
_chemical_name_systematic        dibenzo[b,e]phosphindolizine-P-sulfide
_chemical_temperature_decomposition 453.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-19 deposited with the CCDC.    2019-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.099(2)
_cell_length_b                   12.750(4)
_cell_length_c                   27.638(9)
_cell_measurement_reflns_used    6528
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.4739
_cell_measurement_theta_min      3.1955
_cell_volume                     2501.6(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material
'<i>SHELXL-2014/7</i> and <i>Yadokari-XG 2009</i> (Kabuto <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2014 (Giacovazzo <i>et al.</i>, 2015)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            23615
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         3.195
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9320
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.6094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2747
_reflns_number_total             2849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00463g2.cif
_cod_data_source_block           compound1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as '180 \%C, decomp.'. The value '180 \%C, decomp.' was changed to
'453.15' - it was converted from degrees Celsius(C) to Kelvins(K).

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2501.6(14)
_cod_database_code               7123141
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              47789