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_7118135
_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_formula_moiety
'C83 H54 Cu4 N8 O44 S4, 3.5(C4 H9 N O), 1.5(C H4 O)'
_chemical_formula_sum            'C98.5 H91.5 Cu4 N11.5 O49 S4'
_chemical_formula_weight         2602.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-09-03
_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                90
_cell_angle_beta                 101.20(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.094(3)
_cell_length_b                   20.448(4)
_cell_length_c                   20.371(4)
_cell_measurement_reflns_used    61243
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.948
_cell_measurement_theta_min      1.425
_cell_volume                     6576(2)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_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  0.0645
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61243
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.948
_diffrn_reflns_theta_min         1.425
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             2670
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.754
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         15590
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0719
_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^)+(0.1372P)^2^+10.3495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14130
_reflns_number_total             15590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc07422c2.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C98.50 H91.50 Cu4 N11.50 O49 S4'
_cod_database_code               7118135
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O23-C43
 1.23 with sigma of 0.02
 N7B-C51B
 1.32 with sigma of 0.02
 C52B-C51B = C52A-C51A
 1.5 with sigma of 0.02
 N7A-C54A = N7B-C54B = N7A-C53A = N7B-C53B = N5-C45 = N6-C49 = N6-C50
 1.44 with sigma of 0.02
 O26-C55
 1.4 with sigma of 0.02
 H56A-H2A_$1
 2.2 with sigma of 0.04
 O17_$2-H27A
 2.5 with sigma of 0.04
3. Rigid bond restraints
 O25A, N7A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O25B, N7B, C51B, C52B, C53B, C54B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O27, C56
 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(C53B) \\sim Ueq, Uanis(C54B) \\sim Ueq, Uanis(C53A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H22A(0.25) H22(0.25) C42A(0.25) H42A(0.25) H42B(0.25) H42C(0.25)
 O24(0.5) N6(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C48(0.5) C49(0.5)
 H49A(0.5) H49B(0.5) H49C(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
 O25B(0.25) N7B(0.25) C51B(0.25) C52B(0.25) H52A(0.25) H52B(0.25) H52C(0.25)
 C53B(0.25) H53A(0.25) H53B(0.25) H53C(0.25) C54B(0.25) H54A(0.25) H54B(0.25)
 H54C(0.25) O26(0.5) H26(0.5) C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5) O27(0.25)
 H27A(0.25) C56(0.25) H56A(0.25) H56B(0.25) H56C(0.25) O23(0.5) O25A(0.5)
 N5(0.5) N7A(0.5) C42B(0.25) H42D(0.25) H42E(0.25) H42F(0.25) C43(0.5) C44(0.5)
 H44A(0.5) H44B(0.5) H44C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C46(0.5)
 H46A(0.5) H46B(0.5) H46C(0.5) C51A(0.5) C52A(0.5) H52D(0.5) H52E(0.5)
 H52F(0.5) C53A(0.5) H53D(0.5) H53E(0.5) H53F(0.5) C54A(0.5) H54D(0.5)
 H54E(0.5) H54F(0.5)
6.a Rotating group:
 O21(H21), O22(H22A), O22(H22), O26(H26), O27(H27A)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C19(H19A,H19B), C22(H22B,H22C), C39(H39A,H39B)
6.c Me refined with riding coordinates:
 C42A(H42A,H42B,H42C), C50(H50A,H50B,H50C), C52B(H52A,H52B,H52C), C54B(H54A,
 H54B,H54C), C52A(H52D,H52E,H52F)
6.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C16(H16), C27(H27), C29(H29),
 C30(H30), C32(H32), C33(H33), C36(H36)
6.e Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C53B(H53A,H53B,
 H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C42B(H42D,H42E,H42F),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C53A(H53D,H53E,
 H53F), C54A(H54D,H54E,H54F)
;
_shelx_res_checksum              54385
_shelx_hkl_checksum              7719
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'