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_4135375
_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 Fe2 N24, 4(F6 P), 1.25(C6 H6), C2 H3 N'
_chemical_formula_sum            'C108.5 H94.5 F24 Fe2 N25 P4'
_chemical_formula_weight         2440.17
_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                66.665(2)
_cell_angle_beta                 83.538(2)
_cell_angle_gamma                80.3500(10)
_cell_formula_units_Z            2
_cell_length_a                   14.6717(4)
_cell_length_b                   18.6418(5)
_cell_length_c                   22.0009(4)
_cell_measurement_reflns_used    120722
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     5439.9(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74537
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.912
_diffrn_source                   'Bruker-Nonius FR591 rotating anode'
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.9789
_exptl_absorpt_correction_T_min  0.9192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      x
_exptl_crystal_description       block
_exptl_crystal_F_000             2497
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1571
_refine_ls_number_reflns         19136
_refine_ls_number_restraints     248
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1686
_refine_ls_R_factor_gt           0.1041
_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^)+(0.0002P)^2^+41.8308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.2129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12095
_reflns_number_total             19136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07750_si_005.cif
_cod_data_source_block           '[Fe2L_imid_3][PF6]'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C108.50 H94.50 F24 Fe2 N25 P4'
_cod_database_code               4135375
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.919
_exptl_absorpt_special_details
;
 SADABS was used to perform the Absorption correction
Parameter refinement on 56343 reflections reduced R(int) from 0.1049 to 0.0661
Ratio of minimum to maximum apparent transmission: 0.843604 
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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C802-C801 = C803-C802
 1.39 with sigma of 0.02
 C803_$1-C801 = C803-C801_$1
 1.39 with sigma of 0.02
 C502-C501 = C503-C502 = C504-C503 = C505-C504 = C506-C505 = C506-C501
 1.39 with sigma of 0.02
 C94-C95 \\sim C94-C95A
 with sigma of 0.02
 C95-C99 \\sim C95A-C99A
 with sigma of 0.02
 C95-N24 \\sim C95A-N24A
 with sigma of 0.02
 C96-C97 \\sim C96A-C97A
 with sigma of 0.02
 C96-N24 \\sim C96A-N24A
 with sigma of 0.02
 C97-C98 \\sim C97A-C98A
 with sigma of 0.02
 C98-C99 \\sim C98A-C99A
 with sigma of 0.02
 C94-C99 \\sim C94-C99A
 with sigma of 0.04
 C94-N24 \\sim C94-N24A
 with sigma of 0.04
 C95-C96 \\sim C95A-C96A
 with sigma of 0.04
 C95-C98 \\sim C95A-C98A
 with sigma of 0.04
 C96-C98 \\sim C96A-C98A
 with sigma of 0.04
 C97-C99 \\sim C97A-C99A
 with sigma of 0.04
 C97-N24 \\sim C97A-N24A
 with sigma of 0.04
 C99-N24 \\sim C99A-N24A
 with sigma of 0.04
3. Rigid bond restraints
 C95, N24, C96, C97, C98, C99, C95A, N24A, C96A, C97A, C98A, C99A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C701, C702
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C95 \\sim N24 \\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C95A \\sim N24A
\\sim C96A \\sim C97A \\sim C98A \\sim C99A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C801) \\sim Ueq, Uanis(C802) \\sim Ueq, Uanis(C803) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
5. Others
 Sof(H94C)=Sof(H94D)=Sof(C95A)=Sof(C96A)=Sof(H96A)=Sof(C97A)=Sof(H97A)=
 Sof(C98A)=Sof(H98A)=Sof(C99A)=Sof(H99A)=Sof(N24A)=1-FVAR(1)
 Sof(H94A)=Sof(H94B)=Sof(C95)=Sof(C96)=Sof(H96)=Sof(C97)=Sof(H97)=Sof(C98)=
 Sof(H98)=Sof(C99)=Sof(H99)=Sof(N24)=FVAR(1)
 Sof(C701)=Sof(C702)=Sof(H70C)=Sof(H70D)=Sof(H70E)=Sof(N701)=1-FVAR(2)
 Sof(C601)=Sof(C602)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(N601)=FVAR(2)
 Fixed Sof: C801(0.5) H801(0.5) C802(0.5) H802(0.5) C803(0.5) H803(0.5)
6.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), C94(H94C,H94D)
6.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), C96A(H96A), C97A(H97A), C98A(H98A),
 C99A(H99A), C501(H501), C502(H502), C503(H503), C504(H504), C505(H505),
 C506(H506), C801(H801), C802(H802), C803(H803)
6.c Idealised Me refined as rotating group:
 C602(H60A,H60B,H60C), C702(H70C,H70D,H70E)
;
_shelx_res_checksum              30543
_shelx_hkl_checksum              12543
_olex2_submission_special_instructions 'No special instructions were received'