Self-selecting homochiral quadruple-stranded helicates and control of supramolecular chirality.
Boer, Stephanie A.; Turner, David R.; Chemical communications (Cambridge, England) 51 (2015) 17375–17378; doi:10.1039/c5cc07422c

data_7118131
_publ_section_title
;
 Self-selecting homochiral quadruple-stranded helicates and control of
 supramolecular chirality.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              17375
_journal_page_last               17378
_journal_paper_doi               10.1039/c5cc07422c
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety
'C115.5 H118 Cu4 N8.5 O43.5 S4, 4(C4 H9 N1 O1)'
_chemical_formula_sum            'C131.5 H156 Cu4 N12.5 O47.5 S4'
_chemical_formula_weight         3054.08
_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   mixed
_audit_creation_date             2015-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-03 deposited with the CCDC.
2015-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                113.6200(19)
_cell_angle_beta                 107.650(4)
_cell_angle_gamma                90.700(7)
_cell_formula_units_Z            1
_cell_length_a                   15.702(3)
_cell_length_b                   15.7140(12)
_cell_length_c                   18.656(3)
_cell_measurement_reflns_used    132655
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.966
_cell_measurement_theta_min      2.133
_cell_volume                     3971.6(10)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            132655
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.966
_diffrn_reflns_theta_min         2.133
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            blue
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
Voids 1, 5 and 6 are exterior to the cage. The remaining voids are within the cage.
Appears likely to be 1 DMA molecule per cell (on average).
;
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 13597 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1937
_refine_ls_number_reflns         36094
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      2.495
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1346P)^2^+1.4655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.1967
_reflns_Friedel_coverage         0.917
_reflns_friedel_fraction_full    0.919
_reflns_friedel_fraction_max     0.904
_reflns_number_gt                31648
_reflns_number_total             36094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc07422c2.cif
_cod_data_source_block           d-leu_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        3971.6(9)
_cod_original_formula_sum        'C131.50 H156 Cu4 N12.50 O47.50 S4'
_cod_database_code               7118131
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C132-C131 = C110-C109 = C113-C112
 1.5 with sigma of 0.02
 C40-C39 = C39-C38
 1.39 with sigma of 0.02
 H13M-H13P = H12Q-H12T = H12T-H12P
 2.2 with sigma of 0.02
 N9-H9
 0.91 with sigma of 0.02
 O43-H43B = O43-H43A
 0.86 with sigma of 0.001
 N9-C121 = N9-C120
 1.44 with sigma of 0.02
 H44-C117
 1.9 with sigma of 0.02
 H41-C116
 1.9 with sigma of 0.02
 H41-O41
 0.86 with sigma of 0.02
 N11-C130 = N11-C129 = N13_$1-C138_$1 = N13_$1-C137_$1
 1.45 with sigma of 0.02
 C108-C110
 2.5 with sigma of 0.04
3. Rigid bond restraints
 C36, C37, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O47, N12, C131, C132, C133, C134
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C109, C110, C111
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C112, C113, C114
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S2, O15, O16, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C66, C67, C68, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N9, C120, C121
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C118, O42, C119
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O45, N10, C123, C124, C125, C126
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O41, C116
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32, C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O48, N13, C135, C136, C137, C138
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C125) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C120) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C118) \\sim Ueq,
Uanis(C119) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H10A)=Sof(H10B)=Sof(C109)=Sof(H109)=Sof(C110)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C111)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(H10C)=Sof(H10D)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(H11G)=Sof(H11H)=
 Sof(H11I)=Sof(C114)=Sof(H11J)=Sof(H11K)=Sof(H11L)=FVAR(1)
 Sof(O48)=Sof(N13)=Sof(C135)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C136)=Sof(C137)=
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C138)=Sof(H13G)=Sof(H13H)=Sof(H13I)=1-FVAR(2)
 Sof(O49)=Sof(N14)=Sof(C139)=Sof(H13V)=Sof(H13W)=Sof(H13X)=Sof(C140)=Sof(C141)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C142)=Sof(H14D)=Sof(H14E)=Sof(H14F)=FVAR(2)
 Fixed Sof: O43(0.5) H43A(0.5) H43B(0.5) N9(0.5) H9(0.5) C118(0.25) H11S(0.25)
 H11T(0.25) H11U(0.25) C119(0.25) H11V(0.25) H11W(0.25) H11X(0.25) C120(0.5)
 H12A(0.5) H12B(0.5) H12C(0.5) C121(0.5) H12D(0.5) H12E(0.5) H12F(0.5)
6.a Rotating group:
 O43(H43A,H43B)
6.b Ternary CH refined with riding coordinates:
 N9(H9), C2(H2), C4(H4), C23(H23), C25(H25), C30(H30), C32(H32), C51(H51),
 C53(H53), C58(H58), C60(H60), C79(H79), C81(H81), C86(H86), C88(H88),
 C107(H107), C109(H109), C112(H112)
6.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C24(H24A,H24B), C31(H31A,H31B), C52(H52A,H52B), C59(H59A,H59B),
 C80(H80A,H80B), C87(H87A,H87B), C108(H10A,H10B), C108(H10C,H10D)
6.d Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C61(H61A,H61B,
 H61C), C110(H11A,H11B,H11C), C113(H11G,H11H,H11I), C116(H11M,H11N,H11O),
 C118(H11S,H11T,H11U), C119(H11V,H11W,H11X), C120(H12A,H12B,H12C), C121(H12D,
 H12E,H12F), C135(H13A,H13B,H13C), C137(H13D,H13E,H13F), C138(H13G,H13H,H13I),
 C133(H13M,H13N,H13O), C134(H13P,H13Q,H13R), C125(H12J,H12K,H12L), C126(H12M,
 H12N,H12O), C130(H13S,H13T,H13U), C142(H14D,H14E,H14F)
6.e Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C13(H13), C15(H15), C17(H17), C18(H18), C39(H39),
 C40(H40), C42(H42), C43(H43), C45(H45), C46(H46), C67(H67), C68(H68), C70(H70),
  C71(H71), C73(H73), C74(H74), C95(H95), C96(H96), C98(H98), C99(H99),
 C101(H101), C102(H102)
6.f Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C26(H26A,H26B,H26C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C62(H62A,H62B,H62C), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C111(H11D,H11E,H11F),
 C114(H11J,H11K,H11L), C117(H11P,H11Q,H11R), C131(H13J,H13K,H13L), C123(H12G,
 H12H,H12I), C127(H12P,H12Q,H12R), C129(H12S,H12T,H12U), C139(H13V,H13W,H13X),
 C141(H14A,H14B,H14C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              10296
_shelx_hkl_checksum              60018
_shelx_fab_checksum              84158
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'