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_7720780
_publ_section_title
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 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_absolute_configuration ad
_chemical_formula_moiety
'C120 H114 N6 O20 P6 Zr6, 2(Cl), [+ solvents]8[C5H11NO]'
_chemical_formula_sum            'C160 H202 Cl2 N14 O28 P6 Zr6'
_chemical_formula_weight         3573.38
_chemical_name_common            Zr-P2N2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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            8
_cell_length_a                   53.629(9)
_cell_length_b                   22.341(3)
_cell_length_c                   29.820(5)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100
_cell_measurement_theta_max      16.97
_cell_measurement_theta_min      2.21
_cell_volume                     35728(10)
_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
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.2086
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            165892
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        17.270
_diffrn_reflns_theta_max         17.270
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.0317
_exptl_absorpt_correction_T_min  0.0194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1253 before and 0.1029 after correction.
The Ratio of minimum to maximum transmission is 0.6120.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             14784
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         5462
_refine_ls_number_restraints     917
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+174.1122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4413
_reflns_number_total             5462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00536e2.cif
_cod_data_source_block           Zr-P2N2
_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_cell_volume        35729(10)
_cod_database_code               7720780
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58(10)
 0.42(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
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
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Cl2(0.666667) Cl1(0.333333)
5.a Secondary CH2 refined with riding coordinates:
 C41(H41a,H41b), C38(H38a,H38b), C39(H39a,H39b), C23(H23a,H23b), C24(H24a,
 H24b), C40(H40a,H40b)
5.b Aromatic/amide H refined with riding coordinates:
 O3(H3), C13(H13), C15(H15), C14(H14), C11(H11), C12(H12), C59(H59), C58(H58),
 C56(H56), C55(H55), C22(H22), C21(H21), C19(H19), C18(H18), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C37(H37), C36(H36), C34(H34), C33(H33),
 C30(H30), C29(H29), C28(H28), C27(H27), C26(H26), C53(H53), C52(H52), C51(H51),
  C50(H50), C49(H49), C2(H2), C3(H3a), C4(H4), C5(H5), C1(H1), O1(H1a), O2(H2a),
  C10(H10), C6(H6), C7(H7), C8(H8), C9(H9)
5.c Fitted pentagon refined as free rotating group:
 C13(C15,C14,C11,C12), C2(C3,C4,C5,C1), C10(C6,C7,C8,C9)
5.d Fitted hexagon refined as free rotating group:
 C54(C59,C58,C57,C56,C55), C17(C22,C21,C20,C19,C18), C42(C43,C44,C45,C46,C47),
 C32(C37,C36,C35,C34,C33), C25(C30,C29,C28,C27,C26), C48(C53,C52,C51,C50,C49)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'