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_7132672
_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         'C46 H66 Co2 N18 O10 P4'
_chemical_formula_sum            'C46 H66 Co2 N18 O10 P4'
_chemical_formula_weight         1272.90
_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     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2h09c6
_audit_creation_date             2023-11-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-10 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2983(7)
_cell_length_b                   10.2366(5)
_cell_length_c                   22.8341(12)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.59
_cell_volume                     2864.7(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker AXS Inc., 2018)'
_computing_data_collection       'APEX4 (Bruker AXS Inc., 2021)'
_computing_data_reduction        'SAINT V8.40A (Bruker AXS Inc., 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1306
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            79685
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         1.952
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1061 before and 0.0764 after correction.
The Ratio of minimum to maximum transmission is 0.8385.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         5643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0337P)^2^+11.0044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3802
_reflns_number_total             5643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05804b2.cif
_cod_data_source_block           mo_2022_08_30_jdm_sc_ms_108_0m_a
_cod_depositor_comments
'Adding full bibliography for 7132669--7132673.cif.'
_cod_database_code               7132672
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.901
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23B)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23A)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Fixed Sof: C10B(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C11B(0.5) H11A(0.5)
 H11B(0.5) H11C(0.5) C13B(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C12B(0.5)
 H12A(0.5) H12B(0.5) H12C(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) H9BC(0.5) C8B(0.5)
 H8BA(0.5) H8BB(0.5) H8BC(0.5) N3B(0.5) N6B(0.5) N4B(0.5) N7B(0.5) N5B(0.5)
 N8B(0.5) N4A(0.5) N7A(0.5) N5A(0.5) N8A(0.5) N3A(0.5) N6A(0.5) C10A(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C8A(0.5)
 H8AA(0.5) H8AB(0.5) H8AC(0.5) C12A(0.5) H12D(0.5) H12E(0.5) H12F(0.5)
 C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C13A(0.5) H13D(0.5) H13E(0.5) H13F(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C15(H15), C16(H16), C18(H18), C19(H19),
 C21A(H21A), C21B(H21B)
3.b Idealised Me refined as rotating group:
 C10B(H10A,H10B,H10C), C11B(H11A,H11B,H11C), C13B(H13A,H13B,H13C), C12B(H12A,
 H12B,H12C), C9B(H9BA,H9BB,H9BC), C8B(H8BA,H8BB,H8BC), C22A(H22A,H22B,H22C),
 C23A(H23A,H23B,H23C), C10A(H10D,H10E,H10F), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB,
 H8AC), C12A(H12D,H12E,H12F), C11A(H11D,H11E,H11F), C13A(H13D,H13E,H13F),
 C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F)
;
_shelx_res_checksum              89141
_shelx_hkl_checksum              23799
_olex2_submission_special_instructions 'No special instructions were received'