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_4106694
_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 H4 O'
_chemical_formula_sum            'C97 H112 N4 O'
_chemical_formula_weight         1349.91
_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                 106.389(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.4024(7)
_cell_length_b                   8.9759(3)
_cell_length_c                   24.5083(7)
_cell_measurement_reflns_used    3158
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.04
_cell_measurement_theta_min      3.76
_cell_volume                     4094.8(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 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23349
_diffrn_reflns_theta_full        66.80
_diffrn_reflns_theta_max         66.80
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.9837
_exptl_absorpt_correction_T_min  0.9199
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_description       prism
_exptl_crystal_F_000             1460
_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          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
One methanol per macrocycle
;
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.059
_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   0.977
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1070
_refine_ls_number_reflns         7383
_refine_ls_number_restraints     705
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0891
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1756P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2339
_refine_ls_wR_factor_ref         0.2609
_reflns_number_gt                4283
_reflns_number_total             7383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204795q_si_001_2.cif
_cod_data_source_block           2aMeOH
_cod_database_code               4106694