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_4026063
_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, 1.42C3 H8 O, 0.08H2 O'
_chemical_formula_sum            'C45.28 H80.47 N11 O13.5'
_chemical_formula_weight         994.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 102.360(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   36.417(12)
_cell_length_b                   13.382(5)
_cell_length_c                   11.873(4)
_cell_measurement_reflns_used    9046
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      1.88
_cell_volume                     5652(3)
_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      110(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22959
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9913
_exptl_absorpt_correction_T_min  0.8282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             2149
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         6015
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0594P)^2^+1.9143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                5298
_reflns_number_total             6015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101670a_si_002.cif
_cod_data_source_block           cyclic
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C45.28 H80.47 N11 O13.50'
_cod_database_code               4026063