Self-Assembly of Enantiopure Pd12 Tetrahedral Homochiral Nano-Cages with Tetrazole Linkers and Chiral Recognition.
Howlader, Prodip; Zangrando, Ennio; Mukherjee, Partha Sarathi; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c03551

data_4134854
_publ_section_title
;
 Self-Assembly of Enantiopure Pd12 Tetrahedral Homochiral Nano-Cages with
 Tetrazole Linkers and Chiral Recognition.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c03551
_journal_year                    2020
_chemical_formula_moiety         'C168 H277 N72 Pd12'
_chemical_formula_sum            'C168 H277 N72 Pd12'
_chemical_formula_weight         4582.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.943(5)
_cell_length_b                   25.029(5)
_cell_length_c                   48.678(10)
_cell_measurement_reflns_used    38562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.550
_cell_measurement_theta_min      2.930
_cell_volume                     30390(11)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_collection       'Elettra XRD1 Data Colelction SW'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'rotating crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            244261
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.824
_diffrn_source                   'Elettra Synchrotron, Trieste (Italy)'
_exptl_absorpt_coefficient_mu    0.696
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_description       Block
_exptl_crystal_F_000             9364
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 14143 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.052(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1638
_refine_ls_number_reflns         55917
_refine_ls_number_restraints     2488
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0688P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                38562
_reflns_number_total             55917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03551_si_002.cif
_cod_data_source_block           Lamda_T1
_cod_database_code               4134854
_shelx_shelxl_version_number     2014/7
_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
 C12-C11
 1.5 with sigma of 0.02
 C23-C24
 1.5 with sigma of 0.02
 C13-C12
 1.54 with sigma of 0.02
 C32-C33
 1.54 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Free rotating group:
 N1(N2,C1,C2,C3,C4,C5,C6,C7,C8,C9,C10,N5,N6,C21,C22,C23,C24,C25,C26,C27,C28,
 C29,C30,N7,N8,C31,C32,C33,C34,C35,C36,C37,C38,C39,C40,N9,N10,C41,C42,C43,C44,
 C45,C46,C47,C48,C49,C50,N11,N12,C51,C52,C53,C54,C55,C56,C57,C58,C59,C60,N13,
 N14,C61,C62,C63,C64,C65,C66,C67,C68,C69,C70,N15,N16,C71,C72,C73,C74,C75,C76,
 C77,C78,C79,C80,N17,N18,C81,C82,C83,C85,C86,C87,C88,C89,C90,N19,N20,C91,C92,
 C93,C94,C95,C96,C97,C98,C99,C100,N21,N22,C101,C102,C103,C104,C105,C106,C107,
 C108,C109,C110,N23,N24,C111,C112,C113,C115,C116,C117,C118,C119,C120,N25,N26,
 N27,N28,N29,N30,N31,N32,N33,N34,N35,N36,N37,N38,N39,N40,N41,N42,N43,N44,N45,
 N46,N47,N48,N49,N50,N51,N52,N53,N54,N55,N56,N57,N58,N59,N60,N61,N62,N63,N64,
 N65,N66,N67,N68,N69,N70,N71,N72,C121,C122,C123,C124,C125,C126,C127,C128,C129,
 C130,C131,C132,C133,C134,C135,C136,C137,C138,C139,C140,C141,C142,C143,C144,
 C145,C146,C147,C148,C149,C150,C151,C152,C153,C154,C155,C156,C157,C158,C159,
 C160,C161,C162,C163,C164,C165,C166,C167,C168,C114)
4.b Ternary CH refined with riding coordinates:
 C11(H11), C16(H16), C1(H1), C6(H6), C21(H21), C26(H26), C31(H31), C36(H36),
 C41(H41), C46(H46), C51(H51), C56(H56), C61(H61), C66(H66), C71(H71), C76(H76),
  C81(H81), C86(H86), C91(H91), C96(H96), C101(H101), C106(H106), C111(H111),
 C116(H116)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C15(H15A,H15B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,
 H5B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C52(H52A,H52B),
  C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C62(H62A,H62B), C63(H63A,
 H63B), C64(H64A,H64B), C65(H65A,H65B), C72(H72A,H72B), C73(H73A,H73B),
 C74(H74A,H74B), C75(H75A,H75B), C82(H82A,H82B), C83(H83A,H83B), C85(H85A,H85B),
  C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C102(H10G,
 H10H), C103(H10I,H10J), C104(H10K,H10L), C105(H10M,H10N), C112(H11D,H11E),
 C113(H11F,H11G), C115(H11H,H11I), C114(H11S,H11T), C0AA(H0AA,H0AB), C1AA(H1AA,
 H1AB)
4.d Aromatic/amide H refined with riding coordinates:
 C38(H38), C123(H123), C124(H124), C126(H126), C127(H127), C131(H131),
 C132(H132), C134(H134), C135(H135), C139(H139), C140(H140), C142(H142),
 C143(H143), C147(H147), C148(H148), C150(H150), C151(H151), C155(H155),
 C156(H156), C158(H158), C159(H159), C163(H163), C164(H164), C166(H166),
 C167(H167)
4.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
  C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,
 H79B,H79C), C80(H80A,H80B,H80C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C),
 C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C97(H97A,H97B,H97C), C98(H98A,H98B,
 H98C), C99(H99A,H99B,H99C), C100(H10D,H10E,H10F), C107(H10O,H10P,H10Q),
 C108(H10R,H10S,H10T), C109(H10U,H10V,H10W), C110(H11A,H11B,H11C), C117(H11J,
 H11K,H11L), C118(H11M,H11N,H11O), C119(H11P,H11Q,H11R), C120(H12C,H12D,H12E)
;
_olex2_submission_special_instructions 'No special instructions were received'