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_7159080
_publ_section_title
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 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         '7.7(C H Cl3), C238 H226 N40 O42, [+ solvents]'
_chemical_formula_sum            'C245.7 H233.7 Cl23.69 N40 O42'
_chemical_formula_weight         5258.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-20
_audit_creation_method
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Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2022-12-20 deposited with the CCDC.	2023-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.120(5)
_cell_length_b                   27.450(6)
_cell_length_c                   40.020(8)
_cell_measurement_reflns_used    302550
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.743
_cell_measurement_theta_min      27.743
_cell_volume                     27596(10)
_computing_cell_refinement       'XDS (W. Kabsch, 2010)'
_computing_data_collection       'X-nemo ESRF FIP'
_computing_data_reduction        'XDS (W. Kabsch, 2010)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'ESRF FIP'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.810
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            233506
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.233
_diffrn_reflns_theta_max         25.233
_diffrn_reflns_theta_min         1.252
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       plate
_exptl_crystal_F_000             10906
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.462
_refine_diff_density_min         -2.244
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1343
_refine_ls_number_reflns         15863
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      3.213
_refine_ls_R_factor_all          0.1606
_refine_ls_R_factor_gt           0.1596
_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          0.5440
_refine_ls_wR_factor_ref         0.5480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15547
_reflns_number_total             15863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob02109a2.cif
_cod_data_source_block           dm28
_cod_depositor_comments
'Adding full bibliography for 7159079--7159080.cif.'
_cod_original_formula_sum        'C245.70 H233.70 Cl23.69 N40 O42'
_cod_database_code               7159080
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.917
_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, All O(H) groups
2. Restrained distances
 Cl1_8-Cl2_8
 2.8 with sigma of 0.02
 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
 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
 2.885 with sigma of 0.001
 C22E-C23F
 1.51 with sigma of 0.002
 C8A-C1B
 1.49 with sigma of 0.002
 C2B-C17A
 1.49 with sigma of 0.002
 C4B-C35A
 1.49 with sigma of 0.002
 C1_11-C2_11
 C1_12-C2_12
 C1_13-C2_13
 C1_14-C2_14
 C1_15-C2_15
 C1_16-C2_16
 C1_17-C2_17
 1.51 with sigma of 0.001
 C2_11-C3_11
 C2_12-C3_12
 C2_13-C3_13
 C2_14-C3_14
 C2_15-C3_15
 C2_16-C3_16
 C2_17-C3_17
 1.51 with sigma of 0.001
 C2_11-C4_11
 C2_12-C4_12
 C2_13-C4_13
 C2_14-C4_14
 C2_15-C4_15
 C2_16-C4_16
 C2_17-C4_17
 1.51 with sigma of 0.001
 C3_11-C4_11 = C2_11-?
 C3_12-C4_12 = O1_12-C2_12
 C3_13-C4_13 = O1_13-C2_13
 C3_14-C4_14 = O1_14-C2_14
 C3_15-C4_15 = O1_15-C2_15
 C3_16-C4_16 = O1_16-C2_16
 C3_17-C4_17 = O1_17-C2_17
 2.5 with sigma of 0.02
 O1_12-C1_12
 O1_13-C1_13
 O1_14-C1_14
 O1_15-C1_15
 O1_16-C1_16
 O1_17-C1_17
 1.41 with sigma of 0.01
3. Rigid bond restraints
 C164, N4B, C4B, O4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4_17, C78A, C77A, C79A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5B, C5B, N5B, C41A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3B, C28A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61A, C60A, C59A, C67A, N9A, C66A, C65A, C64A, C63A, C62A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C41A, C5B
 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(Cl05) = Uanis(C162) = Uanis(Cl02) = Uanis(Cl01)
Uiso(Cl3_8) = Uiso(Cl2_10) = Uiso(Cl1_8) = Uiso(Cl1_10) = Uiso(Cl2_8) =
Uiso(Cl3_10)
Uanis(C5A) = Uanis(C4A) = Uanis(C2A) = Uanis(N2A) = Uanis(C7A) = Uanis(C8A) =
Uanis(C3A) = Uanis(C6A) = Uanis(C1A) = Uanis(C9A)
Uanis(O2A) = Uanis(N1A) = Uanis(O1A)
Uiso(C1CL_8) = Uiso(Cl2_8) = Uiso(Cl1_8) = Uiso(Cl3_8) = Uiso(Cl2_9) =
Uiso(Cl3_9) = Uiso(C1CL_9) = Uiso(Cl1_9) = Uiso(Cl1_10) = Uiso(C1CL_10) =
Uiso(Cl2_10) = Uiso(Cl3_10)
Uanis(Cl6) = Uanis(C3) = Uanis(Cl4) = Uanis(Cl5)
Uanis(C4_17) = Uanis(C78A) = Uanis(C77A) = Uanis(C79A)
Uanis(C164) = Uanis(N4B) = Uanis(C4B) = Uanis(O4B) = Uanis(C37A) = Uanis(N6A) =
Uanis(C41A) = Uanis(C40A) = Uanis(C39A) = Uanis(C38A)
5. Rigid body (RIGU) restrains
 C5B, C41A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Cl2)+Sof(C1CL)+Sof(Cl1)+Sof(Cl3)]+1*[Sof(Cl1)+Sof(C1CL)+Sof(Cl2)+
 Sof(Cl3)]+1*[Sof(Cl3)+Sof(C1CL)+Sof(Cl1)+Sof(Cl2)]=1 with esd of 0.001
 Sof(Cl2)=Sof(C1CL)=Sof(Cl1)=Sof(Cl3)=FVAR(1)
 Sof(Cl1)=Sof(C1CL)=Sof(Cl2)=Sof(Cl3)=FVAR(2)
 Sof(Cl3)=Sof(C1CL)=Sof(Cl1)=Sof(Cl2)=FVAR(3)
 Sof(Cl8)=Sof(Cl7)=1-FVAR(4)
 Sof(Cl01)=Sof(Cl02)=Sof(Cl05)=Sof(C162)=Sof(H162)=FVAR(4)
 Sof(C23F)=Sof(C21E)=Sof(C22E)=1-FVAR(5)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=FVAR(5)
7.a Ternary CH refined with riding coordinates:
 C122(H122), C162(H162), C2(H2), C2(H2)
7.b Secondary CH2 refined with riding coordinates:
 C164(H16B,H16C), C1(H1A,H1B), C1(H1A,H1B)
7.c Aromatic/amide H refined with riding coordinates:
 N9B(H9B), N10B(H10B), N3B(H3B), N1B(H1B), N4B(H4B), C79A(H79A), N8B(H8B),
 C74A(H74A), N2B(H2B), N7B(H7B), N5B(H5B), C71A(H71A), C70A(H70A), C25A(H25A),
 C11A(H11A), C7A(H7A), C13A(H13A), N6B(H6B), C16A(H16A), C56A(H56A), C12A(H12A),
  C51A(H51A), C21A(H21A), C69A(H69A), C53A(H53A), C60A(H60A), C20A(H20A),
 C2A(H2A), C29A(H29A), C62A(H62A), C65A(H65A), C42A(H42A), C4A(H4A), C52A(H52A),
  C22A(H22A), C3A(H3A), C43A(H43A), C47A(H47A), C30A(H30A), C31A(H31A),
 C44A(H44A), C38A(H38A), C40A(H40A), C61A(H61A), C34A(H34A), C39A(H39A)
7.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
7.e Idealised tetrahedral OH refined as rotating group:
 O1C(H1C), O2C(H2C)
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_shelx_res_checksum              30134
_shelx_fab_checksum              34497
_olex2_submission_special_instructions 'No special instructions were received'