[4+2] Annulation of arylmethylphosphonochloridates with dibenzo[b,f][1,4]oxazepines: a practical approach to polycyclic benzo-δ-phosphonolactams
Yuan, Xin; Lei, Yelong; Fu, Zhicheng; Xu, Jiaxi; New Journal of Chemistry 47 (2023) 2431–2435; doi:10.1039/D2NJ05558A

data_7062179
_publ_section_title
;
 [4+2] Annulation of arylmethylphosphonochloridates with
 dibenzo[b,f][1,4]oxazepines: a practical approach to polycyclic
 benzo-\d-phosphonolactams
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2431
_journal_page_last               2435
_journal_paper_doi               10.1039/D2NJ05558A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C23 H19 F3 N O3 P'
_chemical_formula_sum            'C23 H19 F3 N O3 P'
_chemical_formula_weight         445.36
_chemical_melting_point          441.1(10)
_chemical_name_common
'dibenzo[b,f]benzo[4,5][1,2]aza-phosphinino[1,6-d][1,4]oxazepine 15-oxide'
_chemical_name_systematic
;
 rel-(4bR,15R)-15-Ethoxy-3-(trifluoromethyl)-4b,16-dihydrodibenzo[b,f]benzo[4,5][1,2]aza-phosphinino[1,6-d][1,4]oxazepine 15-oxide 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-17
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2022-10-10 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.021(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2468(5)
_cell_length_b                   10.0570(5)
_cell_length_c                   16.8219(9)
_cell_measurement_reflns_used    3130
_cell_measurement_temperature    112.35(10)
_cell_measurement_theta_max      28.6920
_cell_measurement_theta_min      3.7470
_cell_volume                     2026.45(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112.35(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0971
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.8380
_diffrn_measurement_details
;
  1 omega   58.00   86.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   57.0000 -150.0000 28

  2 omega   27.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   57.0000 -180.0000 56

  3 omega   49.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  178.0000    0.0000 39

  4 omega   43.00   78.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  178.0000   90.0000 35

  5 omega   31.00   90.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   19.0000  150.0000 59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0424285000
_diffrn_orient_matrix_UB_12      0.0216527000
_diffrn_orient_matrix_UB_13      0.0200266000
_diffrn_orient_matrix_UB_21      -0.0399223000
_diffrn_orient_matrix_UB_22      -0.0378313000
_diffrn_orient_matrix_UB_23      -0.0274730000
_diffrn_orient_matrix_UB_31      0.0106707000
_diffrn_orient_matrix_UB_32      -0.0554352000
_diffrn_orient_matrix_UB_33      0.0265391000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8380
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3971
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+1.2050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                3300
_reflns_number_total             3971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2nj05558a2.cif
_cod_data_source_block           exp_6288
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '167-169 deg' was changed
to '441.1(10)' -- it was converted from degrees Celsius (C) to
kelvins (K), the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7062179.cif.
;
_cod_original_cell_volume        2026.46(17)
_cod_database_code               7062179
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32