Discovery of two predictable (3,18)-connected topologies based on Wells-Dawson type cages for the design of porous metal phosphonocarboxylate frameworks.
Dan, Wenyan; Chen, Zhenxia; Ling, Yun; Jia, Yu; Yang, Yongtai; Liu, Xiaofeng; Deng, Mingli; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7734–7741; doi:10.1039/d4dt00590b

data_7715722
_publ_section_title
;
 Discovery of two predictable (3,18)-connected topologies based on
 Wells-Dawson type cages for the design of porous metal
 phosphonocarboxylate frameworks.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7734
_journal_page_last               7741
_journal_paper_doi               10.1039/d4dt00590b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C102 H86 Co12 N6 O50 P6, 0.167(H12 O6), 11.538(C1.04 H3.813 N0.52)'
_chemical_formula_sum            'C114 H132.01 Co12 N12 O51 P6'
_chemical_formula_weight         3379.29
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2024-04-03 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.208(8)
_cell_length_b                   17.208(8)
_cell_length_c                   40.485(15)
_cell_measurement_reflns_used    990
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.995
_cell_measurement_theta_min      2.432
_cell_volume                     10382(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            16655
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.558
_diffrn_reflns_theta_min         1.697
_exptl_absorpt_coefficient_mu    1.557
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.197211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purle
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       block
_exptl_crystal_F_000             5166
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5097
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0885P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4013
_reflns_number_total             5097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00590b2.cif
_cod_data_source_block           a21101a_a
_cod_depositor_comments
'Adding full bibliography for 7715722--7715727.cif.'
_cod_original_cell_volume        10382(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7715722
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.746
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N2-C18 = N2-C19
 1.45 with sigma of 0.01
 O9-C15 = O9A-C15A
 1.22 with sigma of 0.01
 C15-N1 = C15A-N1A
 1.35 with sigma of 0.01
 N1-C16 = N1-C17 = N1A-C16A = N1A-C17A
 1.45 with sigma of 0.01
 C15-C16 = C15-C17 = C15A-C16A = C15A-C17A
 2.45 with sigma of 0.01
 N2-C18 \\sim N2-C19
 with sigma of 0.01
 N2-C18 \\sim N2A-C18A \\sim N2-C19 \\sim N2A-C19A \\sim N2B-C18B \\sim N2B-C19B
 with sigma of 0.01
 O9A-C15A \\sim O9-C15
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A \\sim C18B-C19B
 with sigma of 0.02
 N1-C15 \\sim N1A-C15A
 with sigma of 0.02
 N1A-C17A \\sim N1A-C16A \\sim N1-C17 \\sim N1-C16
 with sigma of 0.02
 Co2-O9A \\sim Co2-O9
 with sigma of 0.02
 Co2-O1 \\sim Co2A-O1
 with sigma of 0.02
 Co2A-O9 \\sim Co2-O9A
 with sigma of 0.02
3. Restrained planarity
 O9, C15, N1, C16, C17
 with sigma of 0.01
 O9A, C15A, N1A, C17A, C16A
 with sigma of 0.01
 O9, C15, C16, C17, N1
 with sigma of 0.01
 O9A, C15A, C16A, C17A, N1A
 with sigma of 0.01
4. Rigid bond restraints
 N2, C18, C19, N2A, C18A, C19A, N2B, C18B, C19B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9, C15, N1, C16, C17, O9A, C15A, N1A, C16A, C17A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N2 \\sim C18 \\sim C19 \\sim N2A \\sim C18A \\sim C19A \\sim N2B \\sim C18B
\\sim C19B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O9 \\sim C15 \\sim N1 \\sim C16 \\sim C17 \\sim O9A \\sim C15A \\sim N1A \\sim
C16A \\sim C17A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O9 \\sim C15 \\sim N1 \\sim C16 \\sim C17 \\sim O9A \\sim C15A \\sim N1A \\sim
C16A \\sim C17A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(N2) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.12
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9A) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(N1) = Uanis(N1A)
Uanis(Co2A) = Uanis(Co2)
6. Others
 Sof(O9A)=Sof(C15A)=Sof(H15A)=Sof(N1A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(O9)=Sof(C15)=Sof(H15)=Sof(N1)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(Co2A)=1-FVAR(2)
 Sof(Co2)=FVAR(2)
 Fixed Sof: H10A(0.16667) H10B(0.16667) N2(0.52) H2A(0.52) H2B(0.17333)
 C18(0.52) H18A(0.52) H18B(0.52) H18C(0.52) C19(0.52) H19A(0.52) H19B(0.52)
 H19C(0.52) N2A(0.26) H2AA(0.26) H2AB(0.08667) C18A(0.26) H18D(0.26) H18E(0.26)
 H18F(0.26) C19A(0.26) H19D(0.26) H19E(0.26) H19F(0.26) N2B(0.22) H2BA(0.22)
 H2BB(0.07333) C18B(0.22) H18G(0.22) H18H(0.22) H18I(0.22) C19B(0.22)
 H19G(0.22) H19H(0.22) H19I(0.22)
7.a Riding coordinates:
 O10(H10A,H10B)
7.b Ternary CH refined with riding coordinates:
 O8(H8)
7.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N2A(H2AA,H2AB), N2B(H2BA,H2BB)
7.d Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C18A(H18D,H18E,H18F), C19A(H19D,
 H19E,H19F), C18B(H18G,H18H,H18I), C19B(H19G,H19H,H19I), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F)
7.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8A), C10(H10), C12(H12), C15(H15),
 C15A(H15A)
;
_shelx_res_checksum              83560
_olex2_submission_special_instructions 'No special instructions were received'