Putting Cocrystal Stoichiometry to Work: A Reactive Hydrogen-Bonded "Superassembly" Enables Nanoscale Enlargement of a Metal-Organic Rhomboid via a Solid-State Photocycloaddition.
Chu, Qianli; Duncan, Andrew J. E.; Papaefstathiou, Giannis S.; Hamilton, Tamara D.; Atkinson, Manza B. J.; Mariappan, S. V. Santhana; MacGillivray, Leonard R.; Journal of the American Chemical Society 140 (2018) 4940–4944; doi:10.1021/jacs.8b01775

data_4132129
_publ_section_title
;
 Putting Cocrystal Stoichiometry to Work: A Reactive Hydrogen-Bonded
 &quot;Superassembly&quot; Enables Nanoscale Enlargement of a
 Metal-Organic Rhomboid via a Solid-State Photocycloaddition.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4940
_journal_page_last               4944
_journal_paper_doi               10.1021/jacs.8b01775
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '3(C6 H4 Cl2 O2), 2(C18 H14 N2)'
_chemical_formula_sum            'C54 H40 Cl6 N4 O6'
_chemical_formula_weight         1053.60
_chemical_name_common
;
 4,6-diClres,  2-pyr-4-ppyr        
;
_chemical_name_systematic
;
 4,6-dichlororesorcinol, trans-1-(2-pyridyl)-2-(4-(4-phenyl)pyridyl)ethylene)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                85.64(3)
_cell_angle_beta                 80.41(3)
_cell_angle_gamma                65.33(3)
_cell_formula_units_Z            2
_cell_length_a                   11.060(2)
_cell_length_b                   11.180(2)
_cell_length_c                   21.621(4)
_cell_measurement_reflns_used    7944
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     2395.4(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 HKL Denzo, Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15968
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         24.965
_diffrn_reflns_theta_min         2.866
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.937
_exptl_transmission_factor_min   0.806
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         8361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+1.2330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5695
_reflns_number_total             8361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01775_si_002.cif
_cod_data_source_block           3:2assembly
_cod_original_cell_volume        2395.3(10)
_cod_database_code               4132129
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34),
 C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
  C47(H47), C50(H50), C53(H53)
;
_shelx_res_checksum              54522
_shelx_hkl_checksum              82802
_olex2_submission_special_instructions 'No special instructions were received'