Engineering Solid-State Morphologies in Carbazole-Ethynylene Macrocycles
Aaron D. Finke; Dustin E. Gross; Amy Han; Jeffrey S. Moore; Journal of the American Chemical Society 133 (2011) 14063–14070; doi:10.1021/ja204795q

data_4106699
_publ_contact_author
; 
Jeffrey S. Moore 
University of Illinois 
School of Chemical Sciences, Box 55-5 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       jsmoore@illinois.edu
_publ_contact_author_fax         '1  217 244-0181'
_publ_contact_author_phone       '1  217 244 5289'
_publ_section_title
;
 Engineering Solid-State Morphologies in Carbazole-Ethynylene Macrocycles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14063
_journal_page_last               14070
_journal_paper_doi               10.1021/ja204795q
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C92 H100 N4'
_chemical_formula_sum            'C92 H100 N4'
_chemical_formula_weight         1261.76
_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                95.9930(10)
_cell_angle_beta                 98.7200(10)
_cell_angle_gamma                102.3650(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6728(2)
_cell_length_b                   12.2684(2)
_cell_length_c                   15.8148(3)
_cell_measurement_reflns_used    4121
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.02
_cell_measurement_theta_min      3.73
_cell_volume                     1793.72(6)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10274
_diffrn_reflns_theta_full        54.32
_diffrn_reflns_theta_max         54.32
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.9885
_exptl_absorpt_correction_T_min  0.9481
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (? ? ?) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0007(5)
_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   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         4346
_refine_ls_number_restraints     666
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0952
_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^)+(0.1486P)^2^+5.1567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2565
_refine_ls_wR_factor_ref         0.2814
_reflns_number_gt                3160
_reflns_number_total             4346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204795q_si_001_7.cif
_cod_data_source_block           5
_cod_original_cell_volume        1793.71(6)
_cod_database_code               4106699