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_4106693
_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_absolute_configuration unk
_chemical_formula_moiety         'C96 H108 N4, C H2 Cl2'
_chemical_formula_sum            'C97 H110 Cl2 N4'
_chemical_formula_weight         1402.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 105.939(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.3461(6)
_cell_length_b                   8.9264(3)
_cell_length_c                   24.7549(8)
_cell_measurement_reflns_used    8992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.09
_cell_measurement_theta_min      3.39
_cell_volume                     4110.6(2)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_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), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30444
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.8433
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       needle
_exptl_crystal_F_000             1508
_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          0.39
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
One disordered dichloromethane
;
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         7630
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0877
_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^)+(0.1251P)^2^+5.8766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2382
_refine_ls_wR_factor_ref         0.2442
_reflns_number_gt                6608
_reflns_number_total             7630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204795q_si_001_1.cif
_cod_data_source_block           2aDCM
_cod_database_code               4106693