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_4106695
_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         'C96 H108 N4, 2(C H2 Cl2)'
_chemical_formula_sum            'C98 H112 Cl4 N4'
_chemical_formula_weight         1487.72
_chemical_name_systematic
;
 ?
;
_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_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                 105.579(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   42.960(17)
_cell_length_b                   9.082(4)
_cell_length_c                   24.092(10)
_cell_measurement_reflns_used    7438
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.93
_cell_measurement_theta_min      2.26
_cell_volume                     9054(7)
_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), 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      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68724
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.9518
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_description       plate
_exptl_crystal_F_000             3184
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 2 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
Contains 2 disordered dichloromethanes per asymmetric unit.
The voids are extremely large due to "channel" formations that extend
indefinitely along the b-axis.
The actual density of the crystal is higher because of the solvent
in the voids; the reported density reflects the density of the backbone only.
;
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.00126(13)
_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   0.903
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         8238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                4108
_reflns_number_total             8238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204795q_si_001_3.cif
_cod_data_source_block           2b
_cod_original_cell_volume        9055(7)
_cod_database_code               4106695