Fluorescence enhancement via structural rigidification inside a self-assembled Pd4 molecular vessel
Ahmed, Shakil; Howlader, Prodip; Bhattacharyya, Soumalya; Mondal, Surajit; Zangrando, Ennio; Mukherjee, Partha Sarathi; Chemical Communications  (2022) –; doi:10.1039/D2CC04561C

data_7130703
_publ_section_title
;
 Fluorescence enhancement via structural rigidification inside a
 self-assembled Pd4 molecular vessel
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04561C
_journal_year                    2022
_chemical_formula_moiety         'C80 H80 N20 Pd4, 8(N O3), 2(C3 H6 O), O'
_chemical_formula_sum            'C86 H92 N28 O27 Pd4'
_chemical_formula_weight         2375.47
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-06-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-16 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                83.12(3)
_cell_angle_beta                 71.77(3)
_cell_angle_gamma                65.34(3)
_cell_formula_units_Z            2
_cell_length_a                   16.423(3)
_cell_length_b                   18.511(4)
_cell_length_c                   22.079(4)
_cell_measurement_reflns_used    32682
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.99
_cell_measurement_theta_min      2.95
_cell_volume                     5793(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            229558
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.991
_diffrn_reflns_theta_min         0.956
_diffrn_source                   'Elettra Synchrotron, Trieste (Italy)'
_exptl_absorpt_coefficient_mu    0.663
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.572
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1301
_refine_ls_number_reflns         37584
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0808P)^2^+16.7681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32682
_reflns_number_total             37584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04561c2.cif
_cod_data_source_block           MP1
_cod_database_code               7130703
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1A) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103)
\\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C106) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 N13(H13A,H13B), N14(H14A,H14B), N15(H15A,H15B), N16(H16A,H16B), N17(H17A,
 H17B), N18(H18A,H18B), N19(H19A,H19B), N20(H20A,H20B), C81(H81A,H81B),
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B),
  C87(H87A,H87B), C88(H88A,H88B)
3.b Me refined with riding coordinates:
 C101(H10A,H10B,H10C), C103(H10D,H10E,H10F), C104(H10G,H10H,H10I), C106(H10J,
 H10K,H10L)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
  C42(H42), C44(H44), C47(H47), C49(H49), C50(H50), C51(H51), C53(H53),
 C55(H55), C58(H58), C60(H60), C63(H63), C65(H65), C66(H66), C67(H67), C69(H69),
  C71(H71)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56000
_shelx_hkl_checksum              23235
_shelx_fab_checksum              89665
_olex2_submission_special_instructions 'No special instructions were received'