Homochiral coordination cages assembled from dinuclear paddlewheel nodes and enantiopure ditopic ligands: syntheses, structures and catalysis.
Chen, Lianfen; Kang, Jian; Cui, Hao; Wang, Yingxia; Liu, Lan; Zhang, Li; Su, Cheng-Yong; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12180–12188; doi:10.1039/c4dt03782k

data_7034279
_publ_section_title
;
 Homochiral coordination cages assembled from dinuclear paddlewheel nodes
 and enantiopure ditopic ligands: syntheses, structures and catalysis.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12180
_journal_page_last               12188
_journal_paper_doi               10.1039/c4dt03782k
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C100 H121 Cu4 N8 O34, 2(C100 H112 Cu4 N8 O34), 3(O)'
_chemical_formula_sum            'C300 H345 Cu12 N24 O105'
_chemical_formula_weight         6729.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_audit_update_record
;
2015-01-26 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                77.6702(8)
_cell_angle_beta                 78.5238(7)
_cell_angle_gamma                64.3532(10)
_cell_formula_units_Z            1
_cell_length_a                   17.37579(16)
_cell_length_b                   18.2874(2)
_cell_length_c                   32.7446(2)
_cell_measurement_reflns_used    71822
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      64.6570
_cell_measurement_theta_min      3.5850
_cell_volume                     9096.12(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega   -9.00   16.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       32.0000   97.0000 -102.4710 50

  2 omega  -82.00  -14.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -      -39.7748  -38.0000 -180.0000 136

  3 omega -117.00   -6.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -      -39.7748  -77.0000  120.0000 222

  4 omega -120.00  -25.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -      -39.7748  166.0000  153.3955 190

  5 omega -110.00  -79.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -      -39.7748  -19.0000  -60.0000 62

  6 omega  -73.00    6.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -      -39.7748  -19.0000  -60.0000 158

  7 omega -114.00  -10.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -      -39.7748  -57.0000  -60.0000 208

  8 omega  -50.00   36.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -      -39.7748   38.0000   90.0000 172

  9 omega    6.00   31.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       44.0000   90.0000  -21.1909 50

 10 omega   18.00   43.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       52.0000   80.0000   92.7901 50

 11 omega   17.00   42.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       52.0000   82.0000 -163.5486 50

 12 omega   17.00   42.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       52.0000   82.0000  137.7473 50

 13 omega   18.00   43.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       52.0000   80.0000  -97.8438 50

 14 omega   17.00   42.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       52.0000   82.0000   25.0359 50

 15 omega   22.00   47.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       56.0000   78.0000  -47.2604 50

 16 omega   22.00   47.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       56.0000   78.0000  121.0442 50

 17 omega   73.00   99.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000   28.1992 52

 18 omega   30.00   58.00   0.5000    1.6100
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000   28.1992 56

 19 omega   35.00   61.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000  114.2570 52

 20 omega  103.00  136.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000  114.2570 66

 21 omega   38.00   63.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000  154.1925 50

 22 omega  110.00  151.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000  -94.6003 82

 23 omega   38.00   63.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000  -94.6003 50

 24 omega   38.00   63.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000 -166.2780 50

 25 omega   38.00   63.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000  -54.2410 50

 26 omega   38.00   64.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000 -139.7272 52

 27 omega   38.00   64.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000  -28.4731 52

 28 omega  118.00  144.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000  154.1925 52

 29 omega   47.00   72.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       80.0000   75.0000   62.3431 50

 30 omega   86.00  154.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       84.0000   76.0000  -27.9949 136

 31 omega   51.00   77.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       84.0000   76.0000  -27.9949 52

 32 omega   86.00  138.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000 -150.0000 104

 33 omega   55.00   80.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000 -150.0000 50

 34 omega   30.00  105.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408 -125.0000    0.0000 150

 35 omega   87.00  167.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000 -180.0000 160

 36 omega   57.00   83.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000   60.0000 52

 37 omega   55.00   80.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000 -180.0000 50

 38 omega   29.00  120.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408 -125.0000 -180.0000 182

 39 omega   19.00   76.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408  -94.0000   90.0000 114

 40 omega   13.00  122.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408  -77.0000 -180.0000 218

 41 omega   86.00  136.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000  -90.0000 100

 42 omega   55.00   80.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000  -90.0000 50

 43 omega    7.00   92.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408  -94.0000   30.0000 170

 44 omega   85.00  168.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000  120.0000 166

 45 omega   55.00   80.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000   90.0000 50

 46 omega   84.00  137.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000   90.0000 106

 47 omega   55.00   80.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000  120.0000 50

 48 omega   91.00  166.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000    0.0000 150

 49 omega   55.00   88.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000    0.0000 66

 50 omega   90.00  167.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000   60.0000 154

 51 omega   88.00  165.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000   30.0000 154

 52 omega   55.00   80.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000   30.0000 50

 53 omega   55.00   81.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000 -120.0000 52

 54 omega   86.00  165.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000 -120.0000 158

 55 omega   55.00  127.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000  150.0000 144

 56 omega   55.00  144.00   0.5000    6.4600
omega____ theta____ kappa____ phi______ frames
    -       89.1408   77.0000  -60.0000 178
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0467704000
_diffrn_orient_matrix_UB_12      0.0558263000
_diffrn_orient_matrix_UB_13      -0.0021044000
_diffrn_orient_matrix_UB_21      0.0616879000
_diffrn_orient_matrix_UB_22      -0.0659275000
_diffrn_orient_matrix_UB_23      0.0301839000
_diffrn_orient_matrix_UB_31      0.0618361000
_diffrn_orient_matrix_UB_32      -0.0381457000
_diffrn_orient_matrix_UB_33      -0.0379236000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            150437
_diffrn_reflns_point_group_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.987
_diffrn_reflns_theta_min         3.009
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             3501
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 23529 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4063
_refine_ls_number_reflns         58612
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+0.7572P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.858
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                53419
_reflns_number_total             58612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03782k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7034276--7034279.cif.'
_cod_original_cell_volume        9096.12(17)
_cod_database_code               7034279
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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. Rigid bond restraints
 C301, C300
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C299, C298
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(C98B)=1-FVAR(1)
 Sof(C98A)=FVAR(1)
 Fixed Sof: O1A(0.5) O1B(0.5)
4.a Ternary CH refined with riding coordinates:
 C102(H102), C109(H109), C110(H110), C111(H111), C114(H114), C115(H115),
 C116(H116), C119(H119), C126(H126), C133(H133), C134(H134), C135(H135),
 C138(H138), C139(H139), C140(H140), C143(H143), C150(H150), C157(H157),
 C158(H158), C159(H159), C162(H162), C163(H163), C164(H164), C167(H167),
 C174(H174), C181(H181), C182(H182), C183(H183), C186(H186), C188(H188),
 C189(H189), C192(H192), C203(H203), C210(H210), C211(H211), C212(H212),
 C215(H215), C216(H216), C217(H217), C220(H220), C227(H227), C234(H234),
 C235(H235), C236(H236), C239(H239), C240(H240), C241(H241), C244(H244),
 C251(H251), C258(H258), C259(H259), C260(H260), C263(H263), C264(H264),
 C265(H265), C268(H268), C275(H275), C282(H282), C283(H283), C284(H284),
 C287(H287), C288(H288), C289(H289), C292(H292), C2(H2), C9(H9), C10(H10),
 C11(H11), C13(H13), C15(H15), C16(H16), C19(H19), C26(H26), C33(H33), C34(H34),
  C35(H35), C38(H38), C39(H39), C40(H40), C43(H43), C50(H50), C57(H57),
 C58(H58), C59(H59), C62(H62), C63(H63), C64(H64), C67(H67), C74(H74), C81(H81),
  C82(H82), C83(H83), C86(H86), C87(H87), C88(H88), C91(H91)
4.b Secondary CH2 refined with riding coordinates:
 C199(H19J,H19K)
4.c Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C136(H136), C137(H137), C160(H160), C161(H161),
 C184(H184), C185(H185), C198(H198), C213(H213), C214(H214), C237(H237),
 C238(H238), C261(H261), C262(H262), C285(H285), C286(H286), C12(H12), C14(H14),
  C36(H36), C37(H37), C60(H60), C61(H61), C84(H84), C85(H85)
4.d Idealised Me refined as rotating group:
 C104(H10A,H10B,H10C), C105(H10D,H10E,H10F), C106(H10G,H10H,H10I), C122(H12A,
 H12B,H12C), C123(H12D,H12E,H12F), C124(H12G,H12H,H12I), C128(H12J,H12K,H12L),
 C129(H12M,H12N,H12O), C130(H13A,H13B,H13C), C144(H14A,H14B,H14C), C146(H14D,
 H14E,H14F), C147(H14G,H14H,H14I), C151(H15A,H15B,H15C), C153(H15D,H15E,H15F),
 C154(H15G,H15H,H15I), C169(H16A,H16B,H16C), C170(H17A,H17B,H17C), C171(H17D,
 H17E,H17F), C176(H17G,H17H,H17I), C177(H17J,H17K,H17L), C178(H17M,H17N,H17O),
 C194(H19A,H19B,H19C), C195(H19D,H19E,H19F), C196(H19G,H19H,H19I), C200(H20A,
 H20B,H20C), C201(H20D,H20E,H20F), C205(H20G,H20H,H20I), C206(H20J,H20K,H20L),
 C207(H20M,H20N,H20O), C221(H22D,H22E,H22F), C223(H22G,H22H,H22I), C224(H22J,
 H22K,H22L), C229(H22M,H22N,H22O), C230(H23D,H23E,H23F), C231(H23G,H23H,H23I),
 C246(H24A,H24B,H24C), C247(H24D,H24E,H24F), C248(H24G,H24H,H24I), C253(H25A,
 H25B,H25C), C254(H25D,H25E,H25F), C255(H25G,H25H,H25I), C270(H27A,H27B,H27C),
 C271(H27D,H27E,H27F), C272(H27G,H27H,H27I), C277(H27J,H27K,H27L), C278(H27M,
 H27N,H27O), C279(H27P,H27Q,H27R), C295(H29D,H29E,H29F), C296(H29G,H29H,H29I),
 C297(H29J,H29K,H29L), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,
 H71C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C93(H93A,
 H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C)
;
_shelx_res_checksum              38804
_olex2_submission_special_instructions 'No special instructions were received'