Supramolecular Tessellations by a Rigid Naphthalene Diimide Triangle.
Beldjoudi, Yassine; Narayanan, Ashwin; Roy, Indranil; Pearson, Tyler J.; Cetin, M. Mustafa; Nguyen, Minh T.; Krzyaniak, Matthew D.; Alsubaie, Fehaid M.; Wasielewski, Michael R.; Stupp, Samuel I.; Stoddart, J. Fraser; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b08758

data_4127314
_publ_section_title
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 Supramolecular Tessellations by a Rigid Naphthalene Diimide Triangle.
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_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b08758
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety
'3(C20 H14 N2 O4), C1 H0.72 Cl2.56, C0.33 H0.83 Cl0.94, C0.33 H0.83 Cl0.67, C0.33 H0.33 Cl0.93'
_chemical_formula_sum            'C62 H44.71 Cl5.11 N6 O12'
_chemical_formula_weight         1246.97
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2019-07-19 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   26.2442(10)
_cell_length_b                   26.2442(10)
_cell_length_c                   26.2442(10)
_cell_measurement_reflns_used    8157
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.17
_cell_measurement_theta_min      2.92
_cell_volume                     18075.9(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      99.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1175
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54757
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        59.025
_diffrn_reflns_theta_max         59.025
_diffrn_reflns_theta_min         2.916
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.800
_exptl_absorpt_correction_T_max  0.6994
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1357 before and 0.1121 after correction.
The Ratio of minimum to maximum transmission is 0.8470.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       Block
_exptl_crystal_F_000             7699
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.91(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         8600
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0618
_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^)+(0.1132P)^2^+2.6585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                7500
_reflns_number_total             8600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08758_si_009.cif
_cod_data_source_block           yb049_1b
_cod_original_cell_volume        18076(2)
_cod_database_code               4127314
_publcif_datablock.id            {e19d6b44-51bd-4054-a3c0-6436c961fe76}
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.09(3)
 0.91(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Cl1A-C65
 1.77 with sigma of 0.02
4. Others
 Fixed Sof: H61B(0.25) H61C(0.25) H61A(0.25) H61(0.08333) H62(0.08333)
 H62A(0.25) H62C(0.25) H62B(0.25)
5.a Ternary CH refined with riding coordinates:
 C0AA(H0AA), C56(H56), C35(H35), C37(H37), C15(H15), C18(H18), C60(H60),
 C61(H61), C62(H62), C65(H65)
5.b Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C36(H36A,
 H36B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C16(H16A,H16B),
 C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C46(H46), C47(H47), C52(H52), C53(H53), C23(H23), C27(H27), C28(H28),
 C32(H32), C6(H6), C7(H7), C11(H11), C12(H12)
5.d Idealised Me refined as rotating group:
 C61(H61B,H61C,H61A), C62(H62A,H62C,H62B)
;
_shelx_res_checksum              48170
_shelx_hkl_checksum              26932
_shelx_fab_checksum              69422
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
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