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_7132673
_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, 2(C3 H7 N O)'
_chemical_formula_sum            'C52 H80 Co2 N20 O12 P4'
_chemical_formula_weight         1419.10
_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_creation_date             2023-11-10
_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                 92.140(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.5968(15)
_cell_length_b                   10.1687(10)
_cell_length_c                   18.3843(17)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.29
_cell_volume                     3287.3(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker AXS Inc., 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0599
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            110611
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.729
_diffrn_reflns_theta_min         2.217
_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    0.675
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0795 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.9367.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       Shard
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0593P)^2^+5.0380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6922
_reflns_number_total             8525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05804b2.cif
_cod_data_source_block           mo_2023_01_05_jdm_sc_ms275_0m_a
_cod_depositor_comments
'Adding full bibliography for 7132669--7132673.cif.'
_cod_database_code               7132673
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.917
_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, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) H22D(0.5) H22E(0.5) H22F(0.5) H25A(0.5)
 H25B(0.5) H25C(0.5) H25D(0.5) H25E(0.5) H25F(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) H21D(0.5) H21E(0.5) H21F(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 H24D(0.5) H24E(0.5) H24F(0.5) H23A(0.5) H23B(0.5) H23C(0.5) H23D(0.5)
 H23E(0.5) H23F(0.5) N5A(0.5) N6A(0.5) N7A(0.5) N8A(0.5) N9A(0.5) N10A(0.5)
 N5B(0.5) N6B(0.5) N7B(0.5) N8B(0.5) N9B(0.5) N10B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C6(H6), C7(H7), C3(H3), C10(H10), C13(H13), C4(H4),
 C9(H9), C18(H18)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C26(H26D,H26E,H26F), C22(H22A,H22B,H22C), C22(H22D,H22E,
 H22F), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C25(H25D,H25E,H25F), C16(H16A,
 H16B,H16C), C21(H21A,H21B,H21C), C21(H21D,H21E,H21F), C24(H24A,H24B,H24C),
 C24(H24D,H24E,H24F), C23(H23A,H23B,H23C), C23(H23D,H23E,H23F), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              3638
_shelx_hkl_checksum              8478
_olex2_submission_special_instructions 'No special instructions were received'