Lock-Arm Supramolecular Ordering: A Molecular Construction Set for Cocrystallizing Organic Charge Transfer Complexes.
Blackburn, Anthea K.; Sue, Andrew C.-H.; Shveyd, Alexander K.; Cao, Dennis; Tayi, Alok; Narayanan, Ashwin; Rolczynski, Brian S.; Szarko, Jodi M.; Bozdemir, Ozgur A.; Wakabayashi, Rie; Lehrman, Jessica A.; Kahr, Bart; Chen, Lin X.; Nassar, Majed S.; Stupp, Samuel I.; Stoddart, J. Fraser; Journal of the American Chemical Society  (2014) 141124065827003–; doi:10.1021/ja509442t

data_4123056
_publ_section_title
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 Lock-Arm Supramolecular Ordering: A Molecular Construction Set for
 Cocrystallizing Organic Charge Transfer Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141124065827003
_journal_paper_doi               10.1021/ja509442t
_journal_year                    2014
_chemical_formula_moiety         'C18 H20 N2 O8, 0.5(C10 H8 O2)'
_chemical_formula_sum            'C23 H24 N2 O9'
_chemical_formula_weight         472.44
_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             2014-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4866)
;
_cell_angle_alpha                70.8800(10)
_cell_angle_beta                 81.5540(10)
_cell_angle_gamma                83.1560(10)
_cell_formula_units_Z            2
_cell_length_a                   6.78680(10)
_cell_length_b                   10.8904(2)
_cell_length_c                   15.7778(2)
_cell_measurement_reflns_used    5106
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.75
_cell_volume                     1086.72(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16643
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0531P)^2^+0.5751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                4136
_reflns_number_total             6216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja509442t_si_001.cif
_cod_data_source_block           n0478_cs
_cod_database_code               4123056
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.02) H6A(0.024) H6B(0.024) H7A(0.026) H7B(0.026) H8A(0.035)
 H8B(0.035) H9A(0.043) H9B(0.043) H10(0.019) H13A(0.024) H13B(0.024)
 H14A(0.026) H14B(0.026) H16A(0.025) H16B(0.025) H17A(0.029) H17B(0.029)
 H19(0.024) H22(0.022) H23(0.024)
 Fixed X: H2(0.9854) H6A(1.2578) H6B(1.2223) H7A(1.0388) H7B(0.9066)
 H8A(0.621) H8B(0.7701) H9A(0.4796) H9B(0.5426) H10(0.1939) H13A(0.3699)
 H13B(0.1579) H14A(0.6746) H14B(0.6572) H16A(0.2856) H16B(0.3295) H17A(0.9967)
 H17B(0.9387) H19(0.6158) H22(0.5071) H23(0.4217)
 Fixed Y: H2(0.2687) H6A(0.3552) H6B(0.5077) H7A(0.3734) H7B(0.3366)
 H8A(0.4459) H8B(0.4846) H9A(0.633) H9B(0.671) H10(0.9011) H13A(1.1435)
 H13B(1.0892) H14A(1.0801) H14B(0.9924) H16A(0.8747) H16B(0.9615) H17A(1.0098)
 H17B(0.9208) H19(0.6051) H22(0.7281) H23(0.6192)
 Fixed Z: H2(0.5718) H6A(0.2194) H6B(0.1678) H7A(0.1164) H7B(0.2132)
 H8A(0.1296) H8B(0.0377) H9A(0.0306) H9B(0.1121) H10(0.5682) H13A(0.1601)
 H13B(0.2066) H14A(0.1134) H14B(0.0509) H16A(0.2211) H16B(0.1177) H17A(0.0778)
 H17B(0.1798) H19(0.2678) H22(0.5285) H23(0.681)
;
_olex2_submission_special_instructions 'No special instructions were received'