In or out? Adaptive metal binding by a diphosphine-based Zr metal-organic cage
Shin, Jiehye; Wade, Casey R.; Dalton Transactions  (2026) –; doi:10.1039/D6DT00536E

data_7720783
_publ_section_title
;
 In or out? Adaptive metal binding by a diphosphine-based Zr metal-organic
 cage.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6407
_journal_page_last               6414
_journal_paper_doi               10.1039/d6dt00536e
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety
'C122 H119 Ag6 Cl2 N6 O21 P6 S Zr6, C2 H6 O S, 32[C2H6SO], 6[PF6]'
_chemical_formula_sum            'C188 H317 Ag6 Cl2 F36 N6 O54 P12 S34 Zr6'
_chemical_formula_weight         6936.58
_chemical_name_common            Zr-P2N2-Ag_masked_counteranions
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2026-01-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-03-03 deposited with the CCDC.	2026-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0912(14)
_cell_length_b                   40.752(3)
_cell_length_c                   26.4875(19)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      22.39
_cell_measurement_theta_min      2.22
_cell_volume                     22766(3)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2021)'
_computing_data_collection       'APEX5 v2023.9-RC115 (Bruker, 2023)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Photon III area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            321070
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        23.349
_diffrn_reflns_theta_max         23.349
_diffrn_reflns_theta_min         1.834
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.0412
_exptl_absorpt_correction_T_min  0.0217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1107 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.5267.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       block
_exptl_crystal_F_000             14092
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylsulfoxide/ethyl acetate'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.652
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         16843
_refine_ls_number_restraints     962
_refine_ls_restrained_S_all      2.196
_refine_ls_R_factor_all          0.1942
_refine_ls_R_factor_gt           0.1501
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4673
_refine_ls_wR_factor_ref         0.5190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11602
_reflns_number_total             16843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00536e2.cif
_cod_data_source_block           Zr-P2N2-Ag_masked_counteranions
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7720780--7720784.cif.
;
_cod_original_sg_symbol_H-M      Pbcm
_cod_database_code               7720783
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C41-C40
 1.4 with sigma of 0.02
 C40-C39
 1.4 with sigma of 0.02
 C41-C39
 2.3 with sigma of 0.02
 C39-C39_$1
 1.4 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Same fragment restrains
{N3, C60, C61, C62, C63, C64, O6, C59} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N4, C51, C50, C49, C48, C47, O11, C52}
5.a Ternary CH refined with riding coordinates:
 C7(H7), C6(H6)
5.b Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C59(H59A,H59B)
5.c Aromatic/amide H refined with riding coordinates:
 C50(H50), C49(H49), C11(H11), C14(H14), C13(H13), C12(H12), O1(H1), O16(H16),
 O3(H3), O15(H15), C34(H34), C35(H35), C37(H37), C32(H32), C61(H61), C62(H62),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C22(H22), C23(H23), C24(H24),
  C25(H25), C21(H21), C46(H46), C45(H45), C44(H44), C43(H43), C42(H42), C3(H3A),
  C4(H4), C5(H5), C1(H1A), C2(H2), C41(H41), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30), C39(H39), C40(H40)
5.d Fitted pentagon refined as free rotating group:
 C46(C45,C44,C43,C42), C3(C4,C5,C1,C2)
5.e Fitted hexagon refined as free rotating group:
 C10(C11,C14,C15,C13,C12), C34(C35,C36,C37,C32,C33), C53(C54,C55,C56,C57,C58),
 C22(C23,C24,C25,C20,C21), C31(C26,C27,C28,C29,C30)
5.f Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C65(H65A,H65B,H65C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'