Synthesis, structure, and properties of antiaromatic P<sup>V</sup>O complexes of triphyrins(2.1.1).
Sharma, Akrti; Ravikanth, Mangalampalli; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6935–6945; doi:10.1039/d5dt00221d

data_7718491
_publ_section_title
;
 Synthesis, structure, and properties of antiaromatic
 P<sup>V</sup>&#xe001;O complexes of triphyrins(2.1.1).
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6935
_journal_page_last               6945
_journal_paper_doi               10.1039/d5dt00221d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C44 H34 N3 O P'
_chemical_formula_sum            'C44 H34 N3 O P'
_chemical_formula_weight         651.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-09-21 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.590(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1329(6)
_cell_length_b                   13.9091(6)
_cell_length_c                   17.5933(8)
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.8150
_cell_measurement_theta_min      1.9620
_cell_volume                     3419.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'PROGRAM:BIS V6.2.16/2021-10-22 && APEX4 2021.4-0                                '
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -122.88  22.92   1.80    5.00    --  -18.16 -59.25 173.08   81
  2  \w   -122.88  22.92   1.80    5.00    --  -18.16 -59.25  20.08   81
  3  \w   -122.88  22.92   1.80    5.00    --  -18.16 -59.25-135.92   81
  4  \w    -76.17   6.63   1.80    5.00    --  -18.16  89.85 -32.66   46
  5  \w   -122.88  22.92   1.80    5.00    --  -18.16 -59.25  71.08   81
  6  \f   -160.30  26.90   1.80    5.00  72.69 -18.16  31.50    --   104
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0054129000
_diffrn_orient_matrix_UB_12      0.0358203000
_diffrn_orient_matrix_UB_13      0.0277591000
_diffrn_orient_matrix_UB_21      0.0482406000
_diffrn_orient_matrix_UB_22      0.0144085000
_diffrn_orient_matrix_UB_23      0.0002690000
_diffrn_orient_matrix_UB_31      -0.0150389000
_diffrn_orient_matrix_UB_32      0.0333832000
_diffrn_orient_matrix_UB_33      -0.0299119000
_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  0.0893
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52065
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic bluish blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0642P)^2^+2.1732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4750
_reflns_number_total             6018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00221d2.cif
_cod_data_source_block           TPO
_cod_depositor_comments          'Adding full bibliography for 7718491.cif.'
_cod_database_code               7718491
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00U(0.039) H00D(0.038) H00M(0.042) H013(0.043) H00V(0.046)
 H017(0.044) H00F(0.045) H00W(0.051) H00J(0.043) H00C(0.04) H01H(0.081)
 H01I(0.081) H01J(0.081) H014(0.045) H010(0.055) H01D(0.06) H011(0.05)
 H01E(0.113) H01F(0.113) H01G(0.113) H005(0.038) H008(0.042) H00H(0.05)
 H00A(0.047) H01A(0.086) H01B(0.086) H01C(0.086) H012(0.045) H00N(0.051)
 H015(0.054) H00G(0.046) H01K(0.105) H01L(0.105) H01M(0.105)
 Fixed X: H00U(0.967251) H00D(1.012392) H00M(0.763538) H013(0.628266)
 H00V(0.510069) H017(0.617737) H00F(0.931762) H00W(1.017652) H00J(1.040894)
 H00C(0.954876) H01H(1.15092) H01I(1.094041) H01J(1.050049) H014(0.69245)
 H010(0.631876) H01D(0.370892) H011(0.430064) H01E(0.506329) H01F(0.425964)
 H01G(0.405992) H005(0.582359) H008(0.457538) H00H(0.273534) H00A(0.396362)
 H01A(0.292938) H01B(0.216954) H01C(0.25367) H012(0.782733) H00N(0.784814)
 H015(0.822738) H00G(0.819024) H01K(0.738612) H01L(0.811152) H01M(0.851619)
 Fixed Y: H00U(0.441552) H00D(0.330423) H00M(0.261225) H013(0.367828)
 H00V(0.68344) H017(0.66401) H00F(0.186173) H00W(0.050576) H00J(0.153941)
 H00C(0.288827) H01H(0.012838) H01I(-0.046867) H01J(-0.035273) H014(0.60585)
 H010(0.632495) H01D(0.551657) H011(0.525482) H01E(0.627709) H01F(0.548615)
 H01G(0.659326) H005(0.783472) H008(0.890942) H00H(0.705003) H00A(0.597188)
 H01A(0.932536) H01B(0.84749) H01C(0.90655) H012(0.723003) H00N(0.754342)
 H015(0.473099) H00G(0.439961) H01K(0.665377) H01L(0.578224) H01M(0.683819)
 Fixed Z: H00U(0.367974) H00D(0.474571) H00M(0.70245) H013(0.727675)
 H00V(0.433734) H017(0.333441) H00F(0.515559) H00W(0.561867) H00J(0.777368)
 H00C(0.732094) H01H(0.732349) H01I(0.66224) H01J(0.740443) H014(0.781422)
 H010(0.895372) H01D(0.793184) H011(0.679978) H01E(0.971254) H01F(0.944601)
 H01G(0.923191) H005(0.648423) H008(0.653273) H00H(0.53448) H00A(0.529995)
 H01A(0.630207) H01B(0.610561) H01C(0.542554) H012(0.308331) H00N(0.179346)
 H015(0.140881) H00G(0.269701) H01K(0.040071) H01L(0.034394) H01M(0.05573)
;
_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 2.198
_oxdiff_exptl_absorpt_empirical_full_min 0.510