Ring expansion reactions of PO-containing molecules.
Yang, Zhongzhen; Tam, Jerry K. F.; Wootton, Jack M.; Lynam, Jason M.; Unsworth, William P.; Chemical communications (Cambridge, England) 59 (2023) 7927–7930; doi:10.1039/d3cc02087h

data_7131724
_publ_section_title
;
 Ring expansion reactions of P&#xe001;O-containing molecules.
;
_journal_issue                   51
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7927
_journal_page_last               7930
_journal_paper_doi               10.1039/d3cc02087h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C20 H18 N O4 P'
_chemical_formula_sum            'C20 H18 N O4 P'
_chemical_formula_weight         367.32
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-02 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0143(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.34363(18)
_cell_length_b                   9.78579(15)
_cell_length_c                   15.6829(2)
_cell_measurement_reflns_used    6431
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      75.7680
_cell_measurement_theta_min      4.6850
_cell_volume                     1738.49(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  -7.00   0.50    0.15    --  -47.17  59.00-111.00  112
  2  \w   -118.00 -31.00   0.50    0.15    --  -47.17 -59.00 108.00  174
  3  \w     -6.00  20.00   0.50    0.15    --  -47.17  59.00-111.00   52
  4  \w     93.00 178.00   0.50    0.60    --  107.75  59.00-111.00  170
  5  \w     37.00 121.00   0.50    0.60    --  107.75 -59.00 108.00  168
  6  \w      9.00  39.00   0.50    0.15    --   47.17 -59.00 108.00   60
  7  \w     63.00 116.00   0.50    0.15    --   47.17 178.00  30.00  106
  8  \w     67.00  92.00   0.50    0.15    --   47.17 178.00-180.00   50
  9  \w     65.00 120.00   0.50    0.15    --   47.17 178.00 150.00  110
 10  \w     38.00 120.00   0.50    0.60    --  107.75 -37.00-120.00  164
 11  \w     42.00  72.00   0.50    0.60    --  107.75 -99.00-120.00   60
 12  \w     56.00 112.00   0.50    0.60    --  107.75-125.00 120.00  112
 13  \w     76.00 112.00   0.50    0.60    --  107.75 -19.00 -60.00   72
 14  \w     43.00  71.00   0.50    0.60    --  107.75 -19.00 -60.00   56
 15  \w     97.00 168.00   0.50    0.60    --  107.75  19.00-150.00  142
 16  \w     58.00  83.00   0.50    0.60    --  107.75 -99.00-180.00   50
 17  \w     63.00 108.00   0.50    0.60    --  107.75-125.00   0.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0152477000
_diffrn_orient_matrix_UB_12      0.1101106000
_diffrn_orient_matrix_UB_13      -0.0698099000
_diffrn_orient_matrix_UB_21      -0.1345948000
_diffrn_orient_matrix_UB_22      -0.0020181000
_diffrn_orient_matrix_UB_23      0.0088198000
_diffrn_orient_matrix_UB_31      0.0121395000
_diffrn_orient_matrix_UB_32      0.1125083000
_diffrn_orient_matrix_UB_33      0.0687347000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9824
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.049
_diffrn_reflns_theta_max         67.049
_diffrn_reflns_theta_min         4.696
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       irregular
_exptl_crystal_F_000             768
_exptl_crystal_recrystallization_method
'evaporation of an ethyl acetate solution'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.6828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2842
_reflns_number_total             3108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02087h2.cif
_cod_data_source_block           wpu23008
_cod_depositor_comments          'Adding full bibliography for 7131724.cif.'
_cod_original_cell_volume        1738.49(5)
_cod_database_code               7131724
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H18 N1 O4 P1'
_chemical_oxdiff_usercomment     'Zhongzhen Yang YZZ0306-R1'
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
;
_shelx_res_checksum              99085
_shelx_hkl_checksum              63245
_olex2_date_sample_data_collection 2023-04-27
_olex2_date_sample_submission    2023-04-19
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id YZZ0306-R1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.097
_oxdiff_exptl_absorpt_empirical_full_min 0.932