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_7720781
_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_formula_moiety
'C120 H108 Cl6 N6 O20 P6 Pt3 Zr6, 2(Cl), 2(C5 H11 N O), 7[C5H11NO]'
_chemical_formula_sum            'C130 H130 Cl8 N8 O22 P6 Pt3 Zr6'
_chemical_formula_weight         3758.42
_chemical_name_common            Zr-P2N2-PtCl2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-19
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-03-27 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                   48.134(3)
_cell_length_b                   23.0579(18)
_cell_length_c                   17.7804(14)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    240
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.41
_cell_volume                     19734(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      240
_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       '\f and \w 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  0.0604
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            548029
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.878
_diffrn_reflns_theta_max         24.878
_diffrn_reflns_theta_min         1.909
_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    2.626
_exptl_absorpt_correction_T_max  0.0265
_exptl_absorpt_correction_T_min  0.0079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1210 before and 0.0809 after correction.
The Ratio of minimum to maximum transmission is 0.2981.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             7368
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.969
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         17490
_refine_ls_number_restraints     942
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.1032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+613.1752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2170
_refine_ls_wR_factor_ref         0.2408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13509
_reflns_number_total             17490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00536e2.cif
_cod_data_source_block           Zr-P2N2-PtCl2
_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.
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_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7720781
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.527
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C1_$1 = C1-C2 = C2_$1-C3 = C2-C3 = C1-C2
 1.42 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C3(H3), C41(H41), C39(H39), C40(H40), C2(H2), C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C17(H17A,H17B), C59(H59A,H59B), C31(H31A,H31B), C16(H16A,
 H16B), C52(H52A,H52B), C67(H67A,H67B), C68(H68A,H68B)
4.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C34(H34), C36(H36), C37(H37), C11(H11), C12(H12), C14(H14),
 C15(H15), C61(H61), C54(H54), C58(H58), C57(H57), C56(H56), C55(H55), C21(H21),
  C22(H22), C23(H23), C19(H19), C20(H20), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C6(H6), C5(H5), C4(H4), C8(H8), C7(H7), C50(H50), C62(H62),
  C49(H49), C27(H27), C28(H28), C29(H29), C25(H25), C26(H26), C65(H65)
4.d Fitted pentagon refined as free rotating group:
 C42(C43,C44,C45,C46), C6(C5,C4,C8,C7)
4.e Fitted hexagon refined as free rotating group:
 C32(C33,C34,C35,C36,C37), C10(C11,C12,C13,C14,C15), C54(C53,C58,C57,C56,C55),
 C21(C22,C23,C18,C19,C20), C27(C28,C29,C24,C25,C26)
4.f Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C66(H66A,H66B,H66C)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 1596 electrons were found in a volume of 7878\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
28[C5H11NO], which account for 1568 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'