Solid-State Photopolymerization of a Shape-Persistent Macrocycle with Two 1,8-Diazaanthracene Units in a Single Crystal
Ming Li; A. Dieter Schlüter; Junji Sakamoto; Journal of the American Chemical Society 134 (2012) 11721–11725; doi:10.1021/ja3038905

data_4118268
_publ_contact_author_email       schweizer@org.chem.ethz.ch
_publ_contact_author_name        'B. Schweizer'
_publ_section_title
;
 Solid-State Photopolymerization of a Shape-Persistent Macrocycle with Two
 1,8-Diazaanthracene Units in a Single Crystal
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11721
_journal_page_last               11725
_journal_paper_doi               10.1021/ja3038905
_journal_volume                  134
_journal_year                    2012
_chemical_compound_source        'LOC ETH Zurich'
_chemical_formula_moiety         'C96 H64 Cl12 N6 O2 '
_chemical_formula_sum            'C96 H64 Cl12 N6 O2'
_chemical_formula_weight         1759.044
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 131.595(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5095(8)
_cell_length_b                   29.458(2)
_cell_length_c                   16.5367(8)
_cell_measurement_reflns_used    25071
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.910
_cell_volume                     8200.4(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.02766
_diffrn_orient_matrix_UB_12      -0.05070
_diffrn_orient_matrix_UB_13      -0.01390
_diffrn_orient_matrix_UB_21      -0.00349
_diffrn_orient_matrix_UB_22      0.01069
_diffrn_orient_matrix_UB_23      -0.03203
_diffrn_orient_matrix_UB_31      0.02815
_diffrn_orient_matrix_UB_32      -0.07093
_diffrn_orient_matrix_UB_33      -0.02674
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.251
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13777
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    0.46
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       needle
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          .21
_exptl_crystal_size_mid          .036
_exptl_crystal_size_min          .021
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         6963
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.2157
_refine_ls_R_factor_gt           0.1082
_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^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2309
_refine_ls_wR_factor_ref         0.2884
_reflns_number_gt                3303
_reflns_number_total             6963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3038905_si_004.cif
_cod_data_source_block           global
_cod_original_cell_volume        8200.4(6)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C96 H64 Cl12 N6 O2 '
_cod_database_code               4118268