Control of the Intramolecular [2+2] Photocycloaddition in a Bis-Stilbene Macrocycle
Yuewen Xu; Mark D. Smith; Jeanette A. Krause; Linda S. Shimizu; Journal of Organic Chemistry 74 (2009) 4874–4877; doi:10.1021/jo900443e

data_4024603
_publ_section_title
;
Control of the Intramolecular [2+2] Photocycloaddition in a Bis-Stilbene
Macrocycle
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4874
_journal_page_last               4877
_journal_paper_doi               10.1021/jo900443e
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C34 H32 N4 O2, 2(C2 D6 O S)'
_chemical_formula_sum            'C38 H32 D12 N4 O4 S2'
_chemical_formula_weight         696.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.598(4)
_cell_angle_beta                 73.657(4)
_cell_angle_gamma                89.266(4)
_cell_formula_units_Z            1
_cell_length_a                   7.934(2)
_cell_length_b                   9.003(3)
_cell_length_c                   12.354(3)
_cell_measurement_reflns_used    1326
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.822
_cell_measurement_theta_min      4.006
_cell_volume                     839.5(4)
_computing_cell_refinement       'Bruker SAINT v7.56A'
_computing_data_collection       'Bruker APEX2 v2008.5.0'
_computing_data_reduction        'Bruker SAINT v7.56A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8374
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0574P)^2^+0.6088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                2079
_reflns_number_total             2965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo900443e_si_004.cif
_cod_data_source_block           usca002
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4024603