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_4132128
_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         'C6 H4 Cl2 O2, 2(C18 H14 N2)'
_chemical_formula_sum            'C42 H32 Cl2 N4 O2'
_chemical_formula_weight         695.61
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 93.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.838(4)
_cell_length_b                   7.8317(16)
_cell_length_c                   23.075(5)
_cell_measurement_reflns_used    8817
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.02
_cell_volume                     3399.7(12)
_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 0.953
_diffrn_measured_fraction_theta_max 0.975
_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  0.0757
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19023
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         25.041
_diffrn_reflns_theta_min         3.145
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'clear blank colorless'
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   0.983
_exptl_transmission_factor_min   0.932
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         5879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+2.6280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4091
_reflns_number_total             5879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01775_si_002.cif
_cod_data_source_block           2:1assembly
_cod_database_code               4132128
_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:
 C36(H36), C24(H24), C28(H28), C32(H32), C34(H34), C33(H33), C17(H17),
 C31(H31), C41(H41), C15(H15), C21(H21), C1(H1), C37(H37), C27(H27), C11(H11),
 C16(H16), C26(H26), C10(H10), C42(H42), C18(H18), C12(H12), C39(H39), C40(H40),
  C25(H25), C9(H9), C2(H2), C4(H4), C7(H7), C6(H6), C3(H3)
;
_shelx_res_checksum              11017
_shelx_hkl_checksum              10917
_olex2_submission_special_instructions 'No special instructions were received'