Hydrocarbon constrained peptides ‒ understanding preorganisation and binding affinity
Miles, Jennifer A.; Yeo, David J.; Rowell, Philip; Rodriguez-Marin, Silvia; Pask, Christopher M.; Warriner, Stuart L.; Edwards, Thomas A.; Wilson, Andrew J.; Chem. Sci. 7 (2016) 3694–; doi:10.1039/C5SC04048E

data_1542582
_publ_section_title
;
 Hydrocarbon constrained peptides -- understanding preorganisation and
 binding affinity
;
_journal_issue                   6
_journal_name_full               'Chem. Sci.'
_journal_page_first              3694
_journal_paper_doi               10.1039/C5SC04048E
_journal_volume                  7
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H33 N3 Ni O3'
_chemical_formula_sum            'C32 H33 N3 Ni O3'
_chemical_formula_weight         566.32
_chemical_name_systematic
;
(S)-({2-[1-(benzyl)pyrrolidine-2-carboxamide]-phenyl}phenylmethylene)-(S)-pentenylglycinato-N,N',N?,O}nickel(II) 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4773)
;
_audit_update_record
;
2015-03-31 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.0025(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.07980(8)
_cell_length_b                   21.99770(13)
_cell_length_c                   11.88015(9)
_cell_measurement_reflns_used    16707
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      73.2440
_cell_measurement_theta_min      4.2940
_cell_volume                     2832.25(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1033427000
_diffrn_orient_matrix_UB_12      0.0463035000
_diffrn_orient_matrix_UB_13      -0.0440333000
_diffrn_orient_matrix_UB_21      0.0030207000
_diffrn_orient_matrix_UB_22      -0.0173178000
_diffrn_orient_matrix_UB_23      -0.1250600000
_diffrn_orient_matrix_UB_31      -0.0974695000
_diffrn_orient_matrix_UB_32      -0.0496391000
_diffrn_orient_matrix_UB_33      0.0024580000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21899
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         3.80
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.3233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                9713
_reflns_number_total             10002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04048e2.cif
_cod_data_source_block           dy_pent_bpb_tol_cu_a
_cod_depositor_comments          'Adding full bibliography for 1542582.cif.'
_cod_database_code               1542582
_chemical_oxdiff_formula         C33H33N3O4Ni
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: C35A(0.5) H35A(0.5) C35B(0.5) H35B(0.5) C36A(0.5) H36A(0.5)
 C36B(0.5) H36B(0.5) C37A(0.5) H37A(0.5) C37B(0.5) H37B(0.5) C38A(0.5)
 H38A(0.5) C38B(0.5) H38B(0.5) C39A(0.5) H39A(0.5) C39B(0.5) H39B(0.5)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C28(H28), C46(H46), C68(H68)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C33(H33A,H33B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
  C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C73(H73A,H73B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C35A(H35A), C35B(H35B), C36A(H36A), C36B(H36B), C37A(H37A),
  C37B(H37B), C38A(H38A), C38B(H38B), C39A(H39A), C39B(H39B), C42(H42),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62),
  C63(H63), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79)
3.d X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C41(H41A,H41B)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'