A triple-diazonium reagent for virus crosslinking and the synthesis of an azo-linked molecular cage
He, Lijun; Jiang, Chenyang; Chen, Zhuoyue; Ma, Dejun; Yi, Long; Xi, Zhen; Organic & Biomolecular Chemistry  (2022) –; doi:10.1039/D2OB01583H

data_7158888
_publ_section_title
;
 A triple-diazonium reagent for virus crosslinking and the synthesis of an
 azo-linked molecular cage
;
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB01583H
_journal_year                    2022
_chemical_formula_moiety
'C48 H39 N6 O4 P, 1.27979(C H Cl3), 0.72021(C3 H6 O)'
_chemical_formula_sum            'C51.44 H44.6 Cl3.84 N6 O4.72 P'
_chemical_formula_weight         989.42
_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             2022-06-22
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.673(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7423(4)
_cell_length_b                   15.4301(6)
_cell_length_c                   25.1881(8)
_cell_measurement_reflns_used    5418
_cell_measurement_temperature    112.6(5)
_cell_measurement_theta_max      27.0490
_cell_measurement_theta_min      3.8750
_cell_volume                     4881.9(3)
_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      112.6(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0971
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.8256
_diffrn_measurement_details
;
  1 omega  -53.00   55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       16.2414    0.0000    0.0000 108

  2 omega   34.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       16.2414   77.0000  -30.0000 49

  3 omega    1.00   28.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       16.2414   77.0000  -30.0000 27

  4 omega  -54.00  -25.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0070  106.0000  -22.0000 29

  5 omega  -17.00   12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0070  -99.0000 -150.0000 29

  6 omega  -24.00    5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0070  -99.0000   90.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0280597000
_diffrn_orient_matrix_UB_12      -0.0385867000
_diffrn_orient_matrix_UB_13      0.0085592000
_diffrn_orient_matrix_UB_21      -0.0138524000
_diffrn_orient_matrix_UB_22      -0.0173736000
_diffrn_orient_matrix_UB_23      -0.0263265000
_diffrn_orient_matrix_UB_31      0.0469740000
_diffrn_orient_matrix_UB_32      0.0179511000
_diffrn_orient_matrix_UB_33      -0.0071038000
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25542
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.10
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89341
_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_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2053
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform/Acetone'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         9364
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+4.3311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                6885
_reflns_number_total             9364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2ob01583h2.cif
_cod_data_source_block           exp_8030
_cod_original_cell_volume        4882.0(3)
_cod_original_formula_sum        'C51.44 H44.60 Cl3.84 N6 O4.72 P'
_cod_database_code               7158888
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07