Rigid PN cages as 3-dimensional building blocks for crystalline or amorphous networked materials.
Shayan, Mohsen; Abdollahi, Maryam F.; Lawrence, Mason Chester; Guinand, Etienne C.; Goulet, Maxime; George, Tanner; Masuda, Jason D.; Katz, Michael J.; Laventure, Audrey; Werner-Zwanziger, Ulrike; Chitnis, Saurabh S.; Chemical communications (Cambridge, England) 60 (2024) 2629–2632; doi:10.1039/d3cc05804b

data_7132670
_publ_section_title
;
 Rigid PN cages as 3-dimensional building blocks for crystalline or
 amorphous networked materials.
;
_journal_issue                   19
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2629
_journal_page_last               2632
_journal_paper_doi               10.1039/d3cc05804b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C15 H18.80 N5 O2 P1'
_chemical_formula_sum            'C15 H18.8 N5 O2 P'
_chemical_formula_weight         332.12
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_block_doi                 10.5517/ccdc.csd.cc2h3x3n
_audit_creation_date             2022-05-25
_audit_creation_method           'CRYSTALS_ver_14.61_build_7809 '
_audit_update_record
;
2023-09-26 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                108.6532(12)
_cell_angle_beta                 99.9637(12)
_cell_angle_gamma                113.6479(16)
_cell_formula_units_Z            2
_cell_length_a                   9.04350(15)
_cell_length_b                   10.15596(16)
_cell_length_c                   10.73364(12)
_cell_measurement_reflns_used    12290
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      77.8890
_cell_measurement_theta_min      4.6120
_cell_volume                     802.40(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9820
_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    -16.00  26.00   0.50    0.05    --  -48.57  19.00  90.00   84
  2  \w    -75.00  24.00   0.50    0.05    --  -48.57  88.00 -29.00  198
  3  \w   -117.00 -18.00   0.50    0.20    --  -90.00  88.00 -29.00  198
  4  \w    -65.00 -18.00   0.50    0.20    --  -90.00  61.00 -30.00   94
  5  \w    -34.00  24.00   0.50    0.05    --  -48.57  37.00-120.00  116
  6  \w    -16.00  26.00   0.50    0.05    --  -48.57  19.00-120.00   84
  7  \w    -16.00  26.00   0.50    0.05    --  -48.57  19.00 -30.00   84
  8  \w    -16.00  26.00   0.50    0.05    --  -48.57  19.00  30.00   84
  9  \w   -121.00 -39.00   0.50    0.05    --  -48.57 -37.00 -30.00  164
 10  \w   -120.00 -35.00   0.50    0.05    --  -48.57 -57.00 -60.00  170
 11  \w   -120.00 -35.00   0.50    0.05    --  -48.57 -57.00-120.00  170
 12  \w   -120.00 -27.00   0.50    0.05    --  -48.57 -77.00-180.00  186
 13  \w   -120.00 -35.00   0.50    0.05    --  -48.57 -57.00-150.00  170
 14  \w   -120.00 -27.00   0.50    0.05    --  -48.57 -77.00  60.00  186
 15  \w   -120.00 -35.00   0.50    0.05    --  -48.57 -57.00  90.00  170
 16  \w   -161.00 -75.00   0.50    0.20    --  -90.00 -61.00  30.00  172
 17  \w   -161.00 -68.00   0.50    0.20    --  -90.00 -77.00 -90.00  186
 18  \w   -161.00 -68.00   0.50    0.20    --  -90.00 -77.00 -60.00  186
 19  \w   -161.00 -68.00   0.50    0.20    --  -90.00 -77.00 -30.00  186
 20  \w   -161.00 -69.00   0.50    0.20    --  -90.00 -75.00   4.24  184
 21  \w   -161.00 -69.00   0.50    0.20    --  -90.00 -74.00-150.43  184
 22  \w   -161.00 -68.00   0.50    0.20    --  -90.00 -77.00  60.00  186
 23  \w   -161.00 -68.00   0.50    0.20    --  -90.00 -77.00  90.00  186
 24  \w   -161.00 -69.00   0.50    0.20    --  -90.00 -75.00 125.95  184
 25  \w   -161.00 -71.00   0.50    0.20    --  -90.00 -70.00 153.75  180
 26  \w   -161.00 -74.00   0.50    0.20    --  -90.00 -62.00-130.64  174
 27  \w   -161.00 -79.00   0.50    0.20    --  -90.00 -88.00-145.00  164
 28  \w   -161.00 -83.00   0.50    0.20    --  -90.00 -94.00 -60.00  156
 29  \w   -120.00 -73.00   0.50    0.05    --  -48.57-125.00 -30.00   94
 30  \w     40.00  79.00   0.50    0.20    --  111.50 -61.00 -30.00   78
 31  \w     40.00  79.00   0.50    0.20    --  111.50 -61.00  60.00   78
 32  \w     40.00  79.00   0.50    0.20    --  111.50 -61.00  30.00   78
 33  \w     40.00  79.00   0.50    0.20    --  111.50 -61.00 -90.00   78
 34  \w     40.00  79.00   0.50    0.20    --  111.50 -61.00-150.00   78
 35  \w    101.00 178.00   0.50    0.20    --  111.50  88.00 -29.00  154
 36  \w     95.00 178.00   0.50    0.20    --  111.50 125.00   0.00  166
 37  \w     40.00  79.00   0.50    0.20    --  111.50 -61.00   0.00   78
 38  \w     34.00  95.00   0.50    0.05    --   48.57-125.00  90.00  122
 39  \w     40.00 105.00   0.50    0.20    --  111.50 -94.00 -60.00  130
 40  \w     40.00 111.00   0.50    0.20    --  111.50-125.00-150.00  142
 41  \w     40.00 105.00   0.50    0.20    --  111.50 -94.00-150.00  130
 42  \w     40.00 111.00   0.50    0.20    --  111.50-125.00  30.00  142
 43  \w     40.00 105.00   0.50    0.20    --  111.50 -94.00  30.00  130
 44  \w     40.00 105.00   0.50    0.20    --  111.50 -94.00  90.00  130
 45  \w     40.00 107.00   0.50    0.20    --  111.50-102.00 168.23  134
 46  \w     40.00 105.00   0.50    0.20    --  111.50 -94.00 150.00  130
 47  \w     40.00 105.00   0.50    0.20    --  111.50 -94.00 120.00  130
 48  \w     40.00 105.00   0.50    0.20    --  111.50 -94.00   0.00  130
 49  \w    -21.00  75.00   0.50    0.05    --   48.57 -88.00-145.00  192
 50  \w     40.00 138.00   0.50    0.20    --  111.50 -88.00-145.00  196
 51  \w     40.00 105.00   0.50    0.20    --  111.50 -94.00 -90.00  130
 52  \w    101.00 178.00   0.50    0.20    --  111.50  15.00  60.00  154
 53  \w     96.00 178.00   0.50    0.20    --  111.50  61.00  60.00  164
 54  \w     96.00 178.00   0.50    0.20    --  111.50  61.00  90.00  164
 55  \w    101.00 178.00   0.50    0.20    --  111.50  45.00 120.00  154
 56  \w     90.00 178.00   0.50    0.20    --  111.50  77.00 -30.00  176
 57  \w     90.00 178.00   0.50    0.20    --  111.50  77.00 -90.00  176
 58  \w    101.00 178.00   0.50    0.20    --  111.50  45.00 -60.00  154
 59  \w    101.00 178.00   0.50    0.20    --  111.50  45.00-120.00  154
 60  \w    101.00 178.00   0.50    0.20    --  111.50  45.00-150.00  154
 61  \w    101.00 178.00   0.50    0.20    --  111.50  30.00-180.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0824295000
_diffrn_orient_matrix_UB_12      -0.1054204000
_diffrn_orient_matrix_UB_13      0.0059062000
_diffrn_orient_matrix_UB_21      -0.1316621000
_diffrn_orient_matrix_UB_22      -0.1288573000
_diffrn_orient_matrix_UB_23      -0.1457414000
_diffrn_orient_matrix_UB_31      0.1232623000
_diffrn_orient_matrix_UB_32      0.0773036000
_diffrn_orient_matrix_UB_33      -0.0694034000
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_av_unetI/netI     0.084
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26957
_diffrn_reflns_theta_full        74.3338
_diffrn_reflns_theta_max         79.2401
_diffrn_reflns_theta_min         4.6364
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       chunk
_exptl_crystal_F_000             349.606
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3431
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.0039078
_refine_ls_shift/su_mean         0.0001581
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.82P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1126
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1126
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                3101
_reflns_number_total             3431
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.96
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0486
_oxford_refine_ls_scale          8.0(3)
_oxford_reflns_number_all        3431
_cod_data_source_file            d3cc05804b2.cif
_cod_data_source_block           MS-23-pyr
_cod_depositor_comments
'Adding full bibliography for 7132669--7132673.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C15 H18.80 N5 O2 P1'
_cod_database_code               7132670
_cell_oxdiff_length_a            9.04350(15)
_cell_oxdiff_length_b            10.15596(16)
_cell_oxdiff_length_c            10.73364(12)
_cell_oxdiff_angle_alpha         108.6532(12)
_cell_oxdiff_angle_beta          99.9637(12)
_cell_oxdiff_angle_gamma         113.6479(16)
_cell_oxdiff_volume              802.40(2)
_cell_oxdiff_measurement_reflns_used 12290
_oxdiff_exptl_absorpt_empirical_full_min 0.510
_oxdiff_exptl_absorpt_empirical_full_max 2.271
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
012740efbe82df744cb1f4cf326c20b9c1089407dee
;
_diffrn_oxdiff_digest_hkl
;
01ebe1d891ba021d4f9c5870d7db261a0b8d19
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_theta     74.33
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'P2N8O4C20H28 (NC5H5)2'
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0486
_oxford_refine_ls_wr_factor_all  0.1126