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_7132671
_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 N18 O10 P4 Zn2, 2(C3 H7 N O)'
_chemical_formula_sum            'C52 H80 N20 O12 P4 Zn2'
_chemical_formula_weight         1431.98
_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.cc2h3x1l
_audit_creation_date             2023-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-26 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.7137(4)
_cell_length_b                   10.1405(2)
_cell_length_c                   18.5083(4)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      72.20
_cell_measurement_theta_min      3.38
_cell_volume                     3321.49(12)
_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      200.00
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48110
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.069
_diffrn_reflns_theta_min         3.382
_exptl_absorpt_coefficient_mu    2.405
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6334
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       needle
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.792
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.664
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6237
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.666
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.1352
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3327
_refine_ls_wR_factor_ref         0.4196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3917
_reflns_number_total             6237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05804b2.cif
_cod_data_source_block           ms087_0m_monoa_a
_cod_depositor_comments
'Adding full bibliography for 7132669--7132673.cif.'
_cod_database_code               7132671
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.813
_olex2_refinement_description
;
1. Restrained distances
 P1-N2B \\sim P1-N3B \\sim P1-N4B \\sim P2-N7B \\sim P2-N6B \\sim P2-N5B \\sim
P2-N7A \\sim P2-N6A \\sim P2-
 N5A \\sim P1-N2A \\sim P1-N3A \\sim P1-N4A
 with sigma of 0.02
 N7B-C13B \\sim N7A-C13A \\sim N2A-C8A \\sim N2B-C8B \\sim N5B-C11B \\sim
N5A-C11A \\sim N6B-C12B ~
 N6A-C12A \\sim N4A-C10A \\sim N4B-C10B \\sim N3B-C9B \\sim N3A-C9A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C10A \\sim C10B \\sim C13B \\sim C13A \\sim C8A \\sim C8B \\sim C11B \\sim C11A
\\sim C12A \\sim C12B \\sim C9B \\sim C9A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N3B \\sim N6B \\sim N6A \\sim N4A \\sim N4B \\sim N7B \\sim N5A \\sim N3A \\sim
N2B \\sim N5B \\sim N2A \\sim N7A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
3. Others
 Fixed Sof: N2B(0.5) N3B(0.5) N4B(0.5) N5B(0.5) N6B(0.5) N7B(0.5) C8B(0.5)
 H8BA(0.5) H8BB(0.5) H8BC(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) H9BC(0.5) C10B(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C11B(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
 C12A(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C13B(0.5) H13A(0.5) H13B(0.5)
 H13C(0.5) N5A(0.5) N2A(0.5) N3A(0.5) N4A(0.5) N7A(0.5) N6A(0.5) C8A(0.5)
 H8AA(0.5) H8AB(0.5) H8AC(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C10A(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) C13A(0.5) H13D(0.5) H13E(0.5) H13F(0.5)
 C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C12B(0.5) H12D(0.5) H12E(0.5) H12F(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C15(H15), C16(H16), C18(H18), C19(H19),
 C21(H21), C24(H24)
4.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,
 H9BC), C10B(H10A,H10B,H10C), C11B(H11A,H11B,H11C), C12A(H12A,H12B,H12C),
 C13B(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C8A(H8AA,H8AB,
 H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C13A(H13D,H13E,H13F),
 C11A(H11D,H11E,H11F), C12B(H12D,H12E,H12F)
;
_shelx_res_checksum              1974
_shelx_hkl_checksum              94475
_olex2_submission_special_instructions 'No special instructions were received'