Isolated α-turn and incipient γ-helix
M.Mir, Fatemeh; Crisma, Marco; Toniolo, Claudio; Lubell, William D.; Chemical Science  (2019) –; doi:10.1039/C9SC01683J

data_1551305
_publ_section_title
;
 Isolated \a-turn and incipient \g-helix
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01683J
_journal_year                    2019
_chemical_formula_moiety         'C38 H56 N4 O4, 2(C2 H6 O S)'
_chemical_formula_sum            'C42 H68 N4 O6 S2'
_chemical_formula_weight         789.12
_chemical_name_common            'HCO-(Adm)3-NHtBu bis-DMSO solvate'
_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'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-29 deposited with the CCDC.    2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   9.8603(3)
_cell_length_b                   43.0350(14)
_cell_length_c                   38.9591(12)
_cell_measurement_reflns_used    9479
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.685
_cell_measurement_theta_min      2.663
_cell_volume                     16531.8(9)
_computing_cell_refinement
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2013) V8.38A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            305415
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.798
_diffrn_reflns_theta_min         1.786
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1430 before and 0.0731 after correction. The Ratio of minimum to maximum transmission is 0.8465. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       Plate
_exptl_crystal_F_000             6848
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylsulfoxide'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         19053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0791P)^2^+15.4297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16562
_reflns_number_total             19053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01683j2.cif
_cod_data_source_block           lub125
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1551305
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.698
_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 C(H,H,H,H,H,H) groups
2. Others
 Sof(S1B)=Sof(H2BD)=Sof(H2BE)=Sof(H2BF)=1-FVAR(1)
 Sof(S1)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C9B(H9B), C11B(H11B), C13B(H13B), C16B(H16B), C18B(H18B), C20B(H20B),
 C22B(H22B), C25B(H25B), C27B(H27B), C29B(H29B), C31B(H31B), C34B(H34B),
 C9A(H9A), C11A(H11A), C13A(H13A), C16A(H16A), C18A(H18A), C20A(H20A),
 C22A(H22A), C25A(H25A), C27A(H27A), C29A(H29A), C31A(H31A), C34A(H34A)
3.b Secondary CH2 refined with riding coordinates:
 C10B(H10A,H10B), C12B(H12A,H12B), C14B(H14A,H14B), C15B(H15A,H15B), C17B(H17A,
 H17B), C19B(H19A,H19B), C21B(H21A,H21B), C23B(H23A,H23B), C24B(H24A,H24B),
 C26B(H26A,H26B), C28B(H28A,H28B), C30B(H30A,H30B), C32B(H32A,H32B), C33B(H33A,
 H33B), C35B(H35A,H35B), C10A(H10C,H10D), C12A(H12C,H12D), C14A(H14C,H14D),
 C15A(H15C,H15D), C17A(H17C,H17D), C19A(H19C,H19D), C21A(H21C,H21D), C23A(H23C,
 H23D), C24A(H24C,H24D), C26A(H26C,H26D), C28A(H28C,H28D), C30A(H30C,H30D),
 C32A(H32C,H32D), C33A(H33C,H33D), C35A(H35C,H35D)
3.c Aromatic/amide H refined with riding coordinates:
 N1B(H1B), N3B(H3B), N5B(H5B), N7B(H7B), C1B(H1BA), N1A(H1A), N3A(H3A),
 N5A(H5A), N7A(H7A), C1A(H1AA)
3.d Idealised Me refined as rotating group:
 C36B(H36A,H36B,H36C), C37B(H37A,H37B,H37C), C38B(H38A,H38B,H38C), C36A(H36D,
 H36E,H36F), C37A(H37D,H37E,H37F), C38A(H38D,H38E,H38F), C1(H1C,H1D,H1E),
 C2(H2AA,H2AB,H2AC), C2(H2BD,H2BE,H2BF), C3(H3C,H3D,H3E), C4(H4A,H4B,H4C),
 C5(H5C,H5D,H5E), C6(H6A,H6B,H6C), C7(H7C,H7D,H7E), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              70161
_olex2_exptl_crystal_mounting_method 'mounted on a Mylar Cryoloop'
_olex2_submission_original_sample_id 'WDL-FM-07-3-83 DMSO'
_olex2_submission_special_instructions 'No special instructions were received'