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_4133559
_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, 3.84(C20 H14 O2), 16(B F4)'
_chemical_formula_sum            'C508.8 H317.76 B16 F64 Fe8 N120 O7.68 Pd6'
_chemical_formula_weight         10709.21
_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
_atom_sites_solution_primary     direct
_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                   32.5147(6)
_cell_length_b                   32.5147(6)
_cell_length_c                   37.7674(8)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      64.8951
_cell_measurement_theta_min      3.5845
_cell_volume                     39927.9(13)
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   56.00   89.00   1.0000  340.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   77.0000   30.0000 33

  2 omega   97.00  163.00   1.0000  340.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   77.0000   30.0000 66

  3 omega   13.00   38.00   1.0000  340.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118  -30.0000   60.0000 25

  4 omega   60.00   86.00   1.0000  340.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118  -30.0000   60.0000 26

  5 omega   16.00  118.00   1.0000  340.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118  -61.0000  -90.0000 102

  6 omega   57.00  162.00   1.0000  340.0000
omega____ theta____ kappa____ phi______ frames
    -       88.7118   15.0000  150.0000 105

  7 omega  -47.00   34.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038   38.0000  -90.0000 81

  8 omega  -77.00   -5.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038  125.0000   60.0000 72
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0308838000
_diffrn_orient_matrix_UB_12      0.0134350000
_diffrn_orient_matrix_UB_13      0.0287232000
_diffrn_orient_matrix_UB_21      0.0091647000
_diffrn_orient_matrix_UB_22      -0.0396047000
_diffrn_orient_matrix_UB_23      0.0209843000
_diffrn_orient_matrix_UB_31      0.0347153000
_diffrn_orient_matrix_UB_32      0.0222909000
_diffrn_orient_matrix_UB_33      0.0199814000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            64242
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        64.997
_diffrn_reflns_theta_max         64.997
_diffrn_reflns_theta_min         3.587
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85116
_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    0.891
_exptl_crystal_description       block
_exptl_crystal_F_000             10824
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.075(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         16782
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0624
_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^)+(0.1168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1808
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                9015
_reflns_number_total             16782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            delta-cage-final.cif
_cod_data_source_block           delta-cage_sq
_cod_original_cell_volume        39928.0(17)
_cod_original_formula_sum        'C508.80 H317.76 B16 F64 Fe8 N120 O7.68 Pd6'
_cod_database_code               4133559
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         COHNBFFePd
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.689
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.925(10)
 0.075(10)
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
 C64-C64_$1
 1.47 with sigma of 0.01
 C56-C63
 2.8 with sigma of 0.02
 C55-C58
 2.8 with sigma of 0.02
 C64-C57
 2.8 with sigma of 0.02
 C55-C63
 2.4 with sigma of 0.02
 C64-C58
 2.4 with sigma of 0.02
 C63-C57
 2.4 with sigma of 0.02
 C58-C56
 2.4 with sigma of 0.02
 C57-C55
 2.4 with sigma of 0.02
 C56-C64
 2.4 with sigma of 0.02
 C56-C55
 1.39 with sigma of 0.02
 C55-C64
 1.39 with sigma of 0.02
 C64-C63
 1.39 with sigma of 0.02
 C63-C58
 1.39 with sigma of 0.02
 C58-C57
 1.39 with sigma of 0.02
 C57-C56
 1.39 with sigma of 0.02
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4
 with sigma of 0.02
4. Rigid bond restraints
 C52, C53, C54, C50, C51, N15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C52 \\sim C53 \\sim C54 \\sim C50 \\sim C51 \\sim N15: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: C64(0.96) C57(0.96) H57(0.96) C56(0.96) H56(0.96) C62(0.96)
 H62(0.96) C63(0.96) C58(0.96) C59(0.96) H59(0.96) C60(0.96) H60(0.96)
 C61(0.96) H61(0.96) C55(0.96) O1(0.96) H1A(0.96)
7.a Aromatic/amide H refined with riding coordinates:
 C46(H46), N13(H13), C10(H10), C54(H54), C44(H44), C39(H39), C51(H51), C1(H1),
 C2(H2), C37(H37), C19(H19), C38(H38), C3(H3), C45(H45), C53(H53), C26(H26),
 C27(H27), C52(H52), C15(H15), C20(H20), C21(H21), C16(H16), C28(H28), C17(H17),
  C35(H35), C34(H34), C36(H36), C18(H18), C33(H33), N9(H9), N4(H4), C57(H57),
 C56(H56), C62(H62), C59(H59), C60(H60), C61(H61), C9(H9A), C8(H8)
7.b Fitted hexagon refined as free rotating group:
 C62(C63,C58,C59,C60,C61)
7.c Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_olex2_submission_special_instructions 'No special instructions were received'