Design and Enantioresolution of Homochiral Fe(II)-Pd(II) Coordination Cages from Stereolabile Metalloligands: Stereochemical Stability and Enantioselective Separation.
Hou, Ya-Jun; Wu, Kai; Wei, Zhang-Wen; Li, Kang; Lu, Yu-Lin; Zhu, Cheng-Yi; Wang, Jing-Si; Pan, Mei; Jiang, Ji-Jun; Li, Guang-Qin; Su, Cheng-Yong; Journal of the American Chemical Society 140 (2018) 18183–18191; doi:10.1021/jacs.8b11152

data_4133560
_publ_section_title
;
 Design and Enantioresolution of Homochiral Fe(II)-Pd(II) Coordination
 Cages from Stereolabile Metalloligands: Stereochemical Stability and
 Enantioselective Separation.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18183
_journal_page_last               18191
_journal_paper_doi               10.1021/jacs.8b11152
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C432 H264 Fe8 N120 Pd6, 2.8(C20 H14 O2)'
_chemical_formula_sum            'C488 H303.2 Fe8 N120 O5.6 Pd6'
_chemical_formula_weight         9022.49
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.3616(12)
_cell_length_b                   32.3616(12)
_cell_length_c                   37.4948(19)
_cell_measurement_reflns_used    4906
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      64.8634
_cell_measurement_theta_min      3.2705
_cell_volume                     39267(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   67.00  161.00   1.0000  330.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   45.0000 -120.0000 94

  2 omega   60.00   90.00   1.0000  330.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   77.0000   60.0000 30

  3 omega  120.00  164.00   1.0000  330.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   77.0000   60.0000 44

  4 omega   91.00  150.00   1.0000  330.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   45.0000  -60.0000 59

  5 omega  102.00  157.00   1.0000  330.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118  125.0000 -120.0000 55

  6 omega   68.00  165.00   1.0000  330.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   30.0000  120.0000 97

  7 omega  -26.00    7.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038   38.0000 -150.0000 33

  8 omega  -84.00    9.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038  112.0000 -163.0000 93
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0187637000
_diffrn_orient_matrix_UB_12      -0.0162920000
_diffrn_orient_matrix_UB_13      0.0350656000
_diffrn_orient_matrix_UB_21      0.0399773000
_diffrn_orient_matrix_UB_22      -0.0116815000
_diffrn_orient_matrix_UB_23      -0.0199950000
_diffrn_orient_matrix_UB_31      0.0179249000
_diffrn_orient_matrix_UB_32      0.0430769000
_diffrn_orient_matrix_UB_33      0.0078282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1063
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            63868
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        64.965
_diffrn_reflns_theta_max         64.965
_diffrn_reflns_theta_min         3.273
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.555
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.763
_exptl_crystal_description       block
_exptl_crystal_F_000             9200
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.177(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         16551
_refine_ls_number_restraints     605
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1755
_refine_ls_R_factor_gt           0.1029
_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^)+(0.1904P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2742
_refine_ls_wR_factor_ref         0.3318
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6690
_reflns_number_total             16551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lambda-cage-final.cif
_cod_data_source_block           lambda-cage
_cod_original_cell_volume        39267(4)
_cod_original_formula_sum        'C488 H303.20 Fe8 N120 O5.60 Pd6'
_cod_database_code               4133560
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.700
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.823(19)
 0.177(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C55-C56 = C56-C57 = C57-C58 = C58-C59 = C59-C60
 1.39 with sigma of 0.01
 C60-C61 = C61-C62 = C62-C63 = C63-C64 = C64-C55
 1.39 with sigma of 0.01
 C63-C58
 1.39 with sigma of 0.01
 C55-C57 = C56-C58 = C57-C63 = C58-C64
 2.4 with sigma of 0.01
 C63-C55 = C64-C56
 2.4 with sigma of 0.01
 C58-C60 = C59-C61 = C60-C62
 2.4 with sigma of 0.01
 C61-C63 = C62-C58 = C63-C59
 2.4 with sigma of 0.01
 C55-C58 = C56-C63 = C57-C64
 2.8 with sigma of 0.01
 C58-C61 = C59-C62 = C60-C63
 2.8 with sigma of 0.01
 C31-C24
 2.1 with sigma of 0.02
 C49-C50
 1.45 with sigma of 0.02
 C64-C64_$1
 1.45 with sigma of 0.02
4. Restrained planarity
 C59, C62, C56, C57, C58, C63, C64, C55, O1, C60, C61
 with sigma of 0.1
 C17, C18, C14, C16, N5, C15
 with sigma of 0.1
5. Rigid bond restraints
 N12, C37, C38, C39, C40, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54, C50, C51, C52, C53, N15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18, N5, C17, C16, C15, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7, C28, C27, C26, C25, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, N9, N8, C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Fe1, N1, N2, N6, N7, N11, N12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C19, C20, C21, C22, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32, C33, C34, C35, C36, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N11, C46, C47, C45, C44, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C55, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C1, C2, C3, C4, C12, C5, C6, C7, C8, C9, C10, N1, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
N11 \\sim C46 \\sim C47 \\sim C45 \\sim C44 \\sim C43: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim N10: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
N6 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C30: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
Fe1 \\sim N1 \\sim N2 \\sim N6 \\sim N7 \\sim N11 \\sim N12: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C31 \\sim N9 \\sim N8 \\sim C23 \\sim C24: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
N12 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C48: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
C54 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim N15: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
C18 \\sim N5 \\sim C17 \\sim C16 \\sim C15 \\sim C14: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
N7 \\sim C28 \\sim C27 \\sim C26 \\sim C25 \\sim C29: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
C55 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C12 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10 \\sim N1 \\sim C11: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60) =
Uanis(C61) = Uanis(C62) = Uanis(C63) = Uanis(C64)
7. Others
 Fixed Sof: O1(0.7) H1A(0.7) C55(0.7) C56(0.7) H56(0.7) C57(0.7) H57(0.7)
 C58(0.7) C63(0.7) C64(0.7) C59(0.7) H59(0.7) C60(0.7) H60(0.7) C61(0.7)
 H61(0.7) C62(0.7) H62(0.7)
8.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N9(H9), C37(H37), C38(H38), C39(H39), N14(H14), C1(H1), C2(H2),
 C3(H3), C8(H8), C9(H9A), C10(H10), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34),
  C35(H35), C36(H36), C44(H44), C45(H45), C46(H46), C51(H51), C52(H52),
 C53(H53), C54(H54), C56(H56), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62)
8.b Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_olex2_submission_special_instructions 'No special instructions were received'