Single Crystal to Single Crystal Polymerization of a Self-Assembled Diacetylene Macrocycle Affords Columnar Polydiacetylenes
Xu, Weiwei L.; Smith, Mark D.; Krause, Jeanette A.; Greytak, Andrew B.; Ma, Shuguo; Read, Cory M.; Shimizu, Linda S.; Crystal Growth & Design 14 (2014) 993–; doi:10.1021/cg401380a

data_4510136
_publ_section_title
;
 Single Crystal to Single Crystal Polymerization of a Self-Assembled
 Diacetylene Macrocycle Affords Columnar Polydiacetylenes
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              993
_journal_paper_doi               10.1021/cg401380a
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C28 H20 N4 O4, C H4 O'
_chemical_formula_sum            'C29 H24 N4 O5'
_chemical_formula_weight         508.52
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2012-03-28
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                111.787(3)
_cell_angle_beta                 99.823(3)
_cell_angle_gamma                97.184(3)
_cell_formula_units_Z            1
_cell_length_a                   4.5301(10)
_cell_length_b                   11.579(3)
_cell_length_c                   12.321(3)
_cell_measurement_reflns_used    1695
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.854
_cell_measurement_theta_min      3.575
_cell_volume                     578.7(2)
_computing_cell_refinement       'Bruker SAINT v7.68A'
_computing_data_collection       'Bruker APEX2 v2012.2.0'
_computing_data_reduction        'Bruker SAINT v7.68A'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7750
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.39
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1118 before and 0.0396 after correction.
The Ratio of minimum to maximum transmission is 0.8607.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             266
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2841
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0989
_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^)+(0.1426P)^2^+0.7244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2670
_refine_ls_wR_factor_ref         0.2975
_reflns_number_gt                1937
_reflns_number_total             2841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401380a_si_004.cif
_cod_data_source_block           usca023b
_cod_database_code               4510136