Stapling of a 310-Helix with Click Chemistry
Øyvind Jacobsen; Hiroaki Maekawa; Nien-Hui Ge; Carl Henrik Görbitz; Pål Rongved; Ole Petter Ottersen; Mahmood Amiry-Moghaddam; Jo Klaveness; Journal of Organic Chemistry 76 (2011) 1228–1238; doi:10.1021/jo101670a

data_4026062
_publ_contact_author_address
; 
School of Pharmacy
University of Oslo
P.O.Box 1068 Blindern
N-0316 Oslo, Norway
;
_publ_contact_author_email       oyvind.jacobsen@farmasi.uio.no
_publ_contact_author_fax         '+47 22 85 44 02'
_publ_contact_author_name        '\/Oyvind Jacobsen'
_publ_contact_author_phone       '+47 92 81 83 44'
_publ_section_title
;
 Stapling of a 310-Helix with Click Chemistry
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1228
_journal_page_last               1238
_journal_paper_doi               10.1021/jo101670a
_journal_volume                  76
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C41 H69 N11 O12, 0.792C4 H8 O2, 0.558H2 O'
_chemical_formula_sum            'C44.17 H76.45 N11 O14.15'
_chemical_formula_weight         988.03
_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
_audit_update_record
;
2007-06-07 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.239(12)
_cell_length_b                   18.236(14)
_cell_length_c                   18.655(14)
_cell_measurement_reflns_used    980
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.56
_cell_volume                     5524(7)
_computing_cell_refinement       'SAINT+ (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT+ (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXTL (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      111(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II CCD diffractometer'
_diffrn_measurement_method
'Sets of exposures each taken over 0.5\% \w rotation'
_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  0.6253
_diffrn_reflns_av_sigmaI/netI    0.5471
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31484
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9992
_exptl_absorpt_correction_T_min  0.9102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       plate
_exptl_crystal_F_000             2127
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.009
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0210(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         5383
_refine_ls_number_restraints     684
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.3574
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0529P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1929
_reflns_number_gt                1286
_reflns_number_total             5383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101670a_si_001.cif
_cod_data_source_block           acyclic
_cod_database_code               4026062