Rotaxanating Metallo-supramolecular Nano-cylinder Helicates to Switch DNA Junction Binding
Hooper, Catherine A. J.; Cardo, Lucia; Craig, James S.; Melidis, Lazaros; Garai, Aditya; Egan, Ross T.; Sadovnikova, Viktoriia; Burkert, Florian; Male, Louise; Hodges, Nikolas J.; Browning, Douglas F.; Rosas, Roselyne; Liu, Fengbo; Rocha, Fillipe V.; Lima, Mauro A.; Liu, Simin; Bardelang, David; Hannon, Michael J.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c07750

data_4135374
_publ_section_title
;
 Rotaxanating Metallo-supramolecular Nano-cylinder Helicates to Switch DNA
 Junction Binding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c07750
_journal_year                    2020
_chemical_formula_moiety         'C99 H84 N24 Ni2, 4(F6 P), 2(C6 H6)'
_chemical_formula_sum            'C111 H96 F24 N24 Ni2 P4'
_chemical_formula_weight         2463.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                113.514(3)
_cell_angle_beta                 102.465(3)
_cell_angle_gamma                97.137(4)
_cell_formula_units_Z            2
_cell_length_a                   13.3692(9)
_cell_length_b                   22.2187(16)
_cell_length_c                   22.4798(18)
_cell_measurement_reflns_used    133766
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.91
_cell_volume                     5811.4(8)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3200
_diffrn_reflns_av_unetI/netI     0.4293
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_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            68734
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.892
_diffrn_source                   'Bruker-Nonius FR591 rotating anode'
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.9905
_exptl_absorpt_correction_T_min  0.9766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_meas      x
_exptl_crystal_description       block
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         20086
_refine_ls_number_restraints     1545
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.4031
_refine_ls_R_factor_gt           0.1942
_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^)+127.3824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2928
_refine_ls_wR_factor_ref         0.3900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6212
_reflns_number_total             20086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07750_si_004.cif
_cod_data_source_block           '[Ni2L_imid_3][PF6]'
_cod_database_code               4135374
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
 SADABS was used to perform the Absorption correction
Parameter refinement on 24205 reflections reduced R(int) from 0.1474 to 0.0896
Ratio of minimum to maximum apparent transmission: 0.676975
The given Tmin and Tmax were generated using the SHELX SIZE command.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N8-C29 \\sim N16-C62
 with sigma of 0.02
 N8-C30 \\sim N16-C63
 with sigma of 0.02
 C31-C30 \\sim C64-C63
 with sigma of 0.02
 C32-C31 \\sim C65-C64
 with sigma of 0.02
 C33-C32 \\sim C66-C65
 with sigma of 0.02
 C33-C29 \\sim C66-C62
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.03 and sigma
for terminal atoms of 0.06
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C17(H17A,H17B), C28(H28A,H28B), C37(H37A,H37B), C50(H50A,H50B),
 C61(H61A,H61B), C70(H70A,H70B), C83(H83A,H83B), C94(H94A,H94B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48),
  C49(H49), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C59(H59),
 C60(H60), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76), C78(H78), C79(H79), C81(H81),
 C82(H82), C85(H85), C86(H86), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93),
  C96(H96), C97(H97), C98(H98), C99(H99), C501(H501), C502(H502), C503(H503),
 C504(H504), C505(H505), C506(H506), C601(H601), C602(H602), C603(H603),
 C604(H604), C605(H605), C606(H606)
5.c Fitted hexagon refined as free rotating group:
 C18(C19,C20,C21,C22,C23), C44(C45,C46,C47,C48,C49), C51(C52,C53,C54,C55,C56),
 C84(C85,C86,C87,C88,C89), C501(C502,C503,C504,C505,C506), C601(C602,C603,C604,
 C605,C606)
;
_shelx_res_checksum              93424
_shelx_hkl_checksum              614
_shelx_fab_checksum              97121
_olex2_submission_special_instructions 'No special instructions were received'