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_7715723
_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         'C84 H56 Co12 O50 P6, 10(H2 O)'
_chemical_formula_sum            'C84 H76 Co12 O60 P6'
_chemical_formula_weight         2938.42
_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     direct
_audit_creation_date             2024-04-02
_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                   17.070(5)
_cell_length_b                   17.070(5)
_cell_length_c                   39.806(11)
_cell_measurement_reflns_used    3319
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.680
_cell_measurement_theta_min      2.386
_cell_volume                     10045(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1212
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            19924
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         1.469
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.599
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0708 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.8172.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             4422
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.122
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3941
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.1053
_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          0.2877
_refine_ls_wR_factor_ref         0.3460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2090
_reflns_number_total             3941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00590b2.cif
_cod_data_source_block           mo_50104b_0m_a
_cod_depositor_comments
'Adding full bibliography for 7715722--7715727.cif.'
_cod_original_cell_volume        10045(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7715723
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Co1-O1 = Co1A-O1
 2 with sigma of 0.01
 C4-C3A \\sim C3A-C2A \\sim C2A-C1A \\sim C6A-C1A \\sim C6A-C5A \\sim C5A-C4
\\sim C4-C3 \\sim C3-C2 \\sim C2-
 C1 \\sim C6-C1 \\sim C6-C5 \\sim C5-C4
 with sigma of 0.02
 P1-C1A \\sim P1-C1
 with sigma of 0.02
 Co1-O1 \\sim Co1A-O1
 with sigma of 0.02
3. Restrained planarity
 C3, C2, C1, C6, C5, C4
 with sigma of 0.01
 C1A, C2A, C3A, C4, C5A, C6A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C3A \\sim C2A \\sim C1A
\\sim C6A \\sim C5A: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 2A
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Co1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=
 Sof(H3A)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=FVAR(1)
 Sof(Co1A)=1-FVAR(2)
 Sof(Co1)=FVAR(2)
 Fixed Sof: O12(0.5) H12A(0.5) H12B(0.5) O11(0.5) H11A(0.5) H11B(0.5)
 H10A(0.16667) H10B(0.16667) O13(0.25) H13A(0.25) H13B(0.25) O14(0.25)
 H14A(0.25) H14B(0.25)
6.a Riding coordinates:
 O9(H9A,H9B), O12(H12A,H12B), O11(H11A,H11B), O10(H10A,H10B), O13(H13A,H13B),
 O14(H14A,H14B)
6.b Ternary CH refined with riding coordinates:
 O8(H8)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5A(H5A), C6A(H6A), C2A(H2A), C3A(H3A), C5(H5), C6(H6),
 C10(H10), C8(H8A), C12(H12)
6.d Fitted hexagon refined as free rotating group:
 C4(C5A,C6A,C1A,C2A,C3A), C11(C10,C9,C8,C7,C12)
;
_shelx_res_checksum              73758
_olex2_submission_special_instructions 'No special instructions were received'