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_1551301
_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         'C37 H54 N4 O4'
_chemical_formula_sum            'C37 H54 N4 O4'
_chemical_formula_weight         618.84
_chemical_name_common            HCO-(Adm)3-NHiPr
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-03
_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                 109.618(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6491(6)
_cell_length_b                   14.7140(6)
_cell_length_c                   16.1495(7)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    150
_cell_measurement_theta_max      54.240
_cell_measurement_theta_min      2.787
_cell_volume                     3278.9(2)
_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    'ShelXT (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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0774
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.071
_diffrn_reflns_theta_min         2.786
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1175 before and 0.0707 after correction. The Ratio of minimum to maximum transmission is 0.8371. 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    1.254
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1344
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00104(15)
_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   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0584P)^2^+2.0333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3890
_reflns_number_total             6204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01683j2.cif
_cod_data_source_block           lub118
_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               1551301
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.945
_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.a Ternary CH refined with riding coordinates:
 C1B1(H1B1), C1B2(H1B2), C1D1(H1D1), C1D2(H1D2), C2B1(H2B1), C2B2(H2B2),
 C2D1(H2D1), C2D2(H2D2), C3B1(H3B1), C3B2(H3B2), C3D1(H3D1), C3D2(H3D2),
 CT1(HT1)
2.b Secondary CH2 refined with riding coordinates:
 C1G1(H1GA,H1GB), C1G2(H1GC,H1GD), C1G3(H1GE,H1GF), C1G4(H1GG,H1GH), C1E(H1EA,
 H1EB), C2G1(H2GA,H2GB), C2G2(H2GC,H2GD), C2G3(H2GE,H2GF), C2G4(H2GG,H2GH),
 C2E(H2EA,H2EB), C3G1(H3GA,H3GB), C3G2(H3GC,H3GD), C3G3(H3GE,H3GF), C3G4(H3GG,
 H3GH), C3E(H3EA,H3EB)
2.c Aromatic/amide H refined with riding coordinates:
 C0(H0), N1(H1), N2(H2), N3(H3), NT(HT)
2.d Idealised Me refined as rotating group:
 CT2(HT2A,HT2B,HT2C), CT3(HT3A,HT3B,HT3C)
;
_shelx_res_checksum              17368
_olex2_exptl_crystal_mounting_method 'mounted on a Mylar cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'