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_7154089
_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         'C32 H32 F N3 Ni O3, C4 H8 O2'
_chemical_formula_sum            'C36 H40 F N3 Ni O5'
_chemical_formula_weight         672.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
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_cell_angle_beta                 101.348(6)
_cell_angle_gamma                90.00
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_cell_length_b                   14.587(4)
_cell_length_c                   12.850(4)
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_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.159
_cell_measurement_theta_min      2.534
_cell_volume                     1663.9(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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
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_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13122
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
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_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 3954 reflections(SADABS);Rint 0.1397 before
correction and 0.0661 after.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
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_refine_diff_density_max         0.493
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.072(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6380
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                4276
_reflns_number_total             6380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob01832j2.cif
_cod_data_source_block           14079
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        1664.0(8)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7154089