Molecular torsion springs: alteration of helix curvature in frustrated tertiary folds.
Menke, Friedericke S.; Mazzier, Daniela; Wicher, Barbara; Allmendinger, Lars; Kauffmann, Brice; Maurizot, Victor; Huc, Ivan; Organic & biomolecular chemistry 21 (2023) 1275–1283; doi:10.1039/d2ob02109a

data_7159079
_publ_section_title
;
 Molecular torsion springs: alteration of helix curvature in frustrated
 tertiary folds.
;
_journal_issue                   6
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1275
_journal_page_last               1283
_journal_paper_doi               10.1039/d2ob02109a
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C254 H258 N40 O42, 8(C H Cl3)'
_chemical_formula_sum            'C262 H266 Cl24 N40 O42'
_chemical_formula_weight         5497.93
_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             2022-10-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2023-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                105.871(3)
_cell_angle_beta                 95.140(3)
_cell_angle_gamma                114.061(3)
_cell_formula_units_Z            1
_cell_length_a                   18.2180(6)
_cell_length_b                   18.4206(6)
_cell_length_c                   29.4522(10)
_cell_measurement_reflns_used    33179
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      60.9410
_cell_measurement_theta_min      2.7010
_cell_volume                     8450.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku PILATUS conversion'
_diffrn_measurement_method       w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_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       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            85666
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        57.904
_diffrn_reflns_theta_max         57.904
_diffrn_reflns_theta_min         2.706
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       plate
_exptl_crystal_F_000             2862
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.811
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1511
_refine_ls_number_reflns         23289
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.814
_refine_ls_R_factor_all          0.1777
_refine_ls_R_factor_gt           0.1624
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4515
_refine_ls_wR_factor_ref         0.4671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16731
_reflns_number_total             23289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob02109a2.cif
_cod_data_source_block           DM20
_cod_depositor_comments
'Adding full bibliography for 7159079--7159080.cif.'
_cod_original_cell_volume        8450.4(5)
_cod_database_code               7159079
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.658
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1_1-C2_1
 C1_2-C2_2
 C1_3-C2_3
 C1_4-C2_4
 C1_5-C2_5
 C1_6-C2_6
 1.51 with sigma of 0.001
 C2_1-C3_1
 C2_2-C3_2
 C2_3-C3_3
 C2_4-C3_4
 C2_5-C3_5
 C2_6-C3_6
 1.51 with sigma of 0.001
 C2_1-C4_1
 C2_2-C4_2
 C2_3-C4_3
 C2_4-C4_4
 C2_5-C4_5
 C2_6-C4_6
 1.51 with sigma of 0.001
 C3_1-C4_1 = O1_1-C2_1
 C3_2-C4_2 = O1_2-C2_2
 C3_3-C4_3 = O1_3-C2_3
 C3_4-C4_4 = O1_4-C2_4
 C3_5-C4_5 = O1_5-C2_5
 C3_6-C4_6 = O1_6-C2_6
 2.5 with sigma of 0.02
 O1_1-C1_1
 O1_2-C1_2
 O1_3-C1_3
 O1_4-C1_4
 O1_5-C1_5
 O1_6-C1_6
 1.41 with sigma of 0.01
 C1CL_8-Cl1_8 = C1CL_8-Cl2_8 = C1CL_8-Cl3_8
 C1CL_9-Cl1_9 = C1CL_9-Cl2_9 = C1CL_9-Cl3_9
 C1CL_10-Cl1_10 = C1CL_10-Cl2_10 = C1CL_10-Cl3_10
 C1CL_11-Cl1_11 = C1CL_11-Cl2_11 = C1CL_11-Cl3_11
 1.755 with sigma of 0.001
 Cl1_8-Cl2_8 = Cl2_8-Cl3_8 = Cl3_8-Cl1_8
 Cl1_9-Cl2_9 = Cl2_9-Cl3_9 = Cl3_9-Cl1_9
 Cl1_10-Cl2_10 = Cl2_10-Cl3_10 = Cl3_10-Cl1_10
 Cl1_11-Cl2_11 = Cl2_11-Cl3_11 = Cl3_11-Cl1_11
 2.85 with sigma of 0.001
 C2C-C1C = C3C-C1C = C4C-C1C
 1.51 with sigma of 0.002
 C81-C2_6
 1.51 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C4_6) = Uanis(C2_6) = Uanis(C81) = Uanis(C3_6)
4. Others
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(H2B)=1-FVAR(1)
 Sof(H2A)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C027(H027), C2(H2), C2(H2B), C2(H2A), C1CL(H1CL), C1CL(H1CL), C1CL(H1CL),
 C1CL(H1CL)
5.b Secondary CH2 refined with riding coordinates:
 C023(H02A,H02B), C5B(H5BA,H5BB), C1(H1A,H1B), C1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 N8B(H8B), N9B(H9B), N10B(H10B), N5B(H5B), N6B(H6B), N7B(H7B), C66A(H66A),
 C75A(H75A), C70A(H70A), C72A(H72A), C71A(H71A), C79A(H79A), C52A(H52A),
 N3B(H3B), C61A(H61A), N4B(H4B), C48A(H48A), C53A(H53A), C63A(H63A), C43A(H43A),
  C44A(H44A), C57A(H57A), C45A(H45A), C62A(H62A), C54A(H54A), N1B(H1B),
 C40A(H40A), N2B(H2B), C25A(H25A), C29A(H29A), C11A(H11A), C12A(H12A),
 C13A(H13A), C16A(H16A), C34A(H34A), C22A(H22A), C31A(H31A), C39A(H39A),
 C30A(H30A), C21A(H21A), C38A(H38A), C20A(H20A), C2A(H2A), C3A(H3A), C4A(H4A),
 C7A(H7A)
5.d Naphthalene refined as free rotating group:
 C10A(C11A,C12A,C13A,C14A,C18A,N3A,C17A,C16A,C15A), C1A(C2A,C3A,C4A,C5A,C9A,
 N2A,C8A,C7A,C6A)
5.e Idealised Me refined as rotating group:
 C02X(H02C,H02D,H02E), C03Q(H03A,H03B,H03C), C8C(H8CA,H8CB,H8CC), C7C(H7CA,
 H7CB,H7CC), C6C(H6CA,H6CB,H6CC), C81(H81A,H81B,H81C), C3(H3A,H3B,H3C), C4(H4A,
 H4B,H4C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85782
_shelx_fab_checksum              36649
_olex2_submission_special_instructions 'No special instructions were received'