Robust asymmetric synthesis of unnatural alkenyl amino acids for conformationally constrained α-helix peptides.
Aillard, Boris; Robertson, Naomi S.; Baldwin, Adam R.; Robins, Siobhan; Jamieson, Andrew G.; Organic & biomolecular chemistry 12 (2014) 8775–8782; doi:10.1039/c4ob01832j

data_7154088
_publ_section_title
;
 Robust asymmetric synthesis of unnatural alkenyl amino acids for
 conformationally constrained \a-helix peptides.
;
_journal_issue                   43
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8775
_journal_page_last               8782
_journal_paper_doi               10.1039/c4ob01832j
_journal_volume                  12
_journal_year                    2014
_chemical_absolute_configuration ,syn
_chemical_formula_moiety         'C28 H26 F N3 Ni O3,2C H2 Cl2'
_chemical_formula_sum            'C30 H30 Cl4 F N3 Ni O3'
_chemical_formula_weight         700.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1183(19)
_cell_length_b                   14.255(3)
_cell_length_c                   23.374(5)
_cell_measurement_reflns_used    585
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.275
_cell_measurement_theta_min      2.254
_cell_volume                     3038.2(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1504
_diffrn_reflns_av_sigmaI/netI    0.1948
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23982
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 3643 reflections(SADABS);Rint 0.0977 before
correction and 0.0595 after.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;

Disordered CH2Cl2 was omitted using the SQUEEZE option of PLATON.The
solvent accessible voids are 813.0 3 with an estimated 382e/cell to 
be added.Eight solvent CH2Cl2 molecules/unit cell accounting for 336e
were included in the formula, FWt, (000) and density calculations. 
PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34.

;
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5973
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0584P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                3142
_reflns_number_total             5973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob01832j2.cif
_cod_data_source_block           14066
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7154086--7154091.cif.
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7154088