Helical Pitch of m-Phenylene Ethynylene Foldamers by Double Spin Labeling
Kenji Matsuda; Matthew T. Stone; Jeffrey S. Moore; Journal of the American Chemical Society 124 (2002) 11836–11837; doi:10.1021/ja027437m

data_4115190
_publ_contact_author
;
Prof. Jeffrey S. Moore
Roger Adams Laboratory
Departments of Chemistry and Materials Science & Engineering
University of Illinois at Urbana-Champaign
Urbana, Illinois 61801, USA
;
_publ_contact_author_email       ' moore@scs.uiuc.edu'
_publ_contact_author_fax         ' 1(217)2448068 '
_publ_contact_author_phone       ' 1(217)2444024 '
_publ_section_title
;
 Helical Pitch of m-Phenylene Ethynylene Foldamers by Double Spin Labeling
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11836
_journal_page_last               11837
_journal_paper_doi               10.1021/ja027437m
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C20 H23 N2 O2'
_chemical_formula_weight         323.42
_chemical_melting_point          471(2)
_chemical_name_systematic
; 
 3,5-diethynyl-N-(1-oxy-2,2,6,6-tetramethyl-piperidine-4-yl)-benzamide
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            16
_cell_length_a                   30.635(4)
_cell_length_b                   7.7786(10)
_cell_length_c                   30.476(4)
_cell_measurement_reflns_used    987
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      42.8
_cell_measurement_theta_min      5.6
_cell_volume                     7262.4(16)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '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  0.2044
_diffrn_reflns_av_sigmaI/netI    0.1504
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            37753
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_time  397
_diffrn_standards_number         335
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       platy
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          1.15
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1917
_reflns_number_gt                3392
_reflns_number_total             6677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027437m_s2.cif
_cod_data_source_block           2
_cod_database_code               4115190