Diversifying molecular and topological space via a supramolecular solid-state synthesis: a purely organic mok net sustained by hydrogen bonds
Oburn, Shalisa M.; Sinnwell, Michael A.; Ericson, Devin P.; Reinheimer, Eric W.; Proserpio, Davide M.; Groeneman, Ryan H.; MacGillivray, Leonard; IUCrJ 6 (2019) –; doi:10.1107/S2052252519011382

data_1552294
_publ_section_title
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 Diversifying molecular and topological space via a supramolecular
 solid-state synthesis: a purely organic mok net sustained by hydrogen
 bonds
;
_journal_issue                   6
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252519011382
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         '2(C15 H13 N O2), C6 H4 I2 O2'
_chemical_formula_sum            'C36 H30 I2 N2 O6'
_chemical_formula_weight         840.42
_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
_audit_creation_date             2015-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                101.278(5)
_cell_angle_beta                 92.285(5)
_cell_angle_gamma                111.552(5)
_cell_formula_units_Z            2
_cell_length_a                   9.3954(9)
_cell_length_b                   10.055(2)
_cell_length_c                   19.911(2)
_cell_measurement_reflns_used    7232
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.00
_cell_volume                     1702.8(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski and Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1998)'
_computing_data_reduction        'Denzo (Otwinowski and Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD rotation images, phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14414
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.946
_diffrn_reflns_theta_min         1.051
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1061 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.8044.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0592P)^2^+0.1166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4839
_reflns_number_total             8137
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {48007827-d559-4df6-beb4-1e63197ae08e}
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_cod_data_source_file            yc5020.cif
_cod_data_source_block           web134
_cod_database_code               1552294
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C33(H33), C7(H7), C9(H9), C6(H6), C12(H12), C11(H11), C10(H10),
 C27(H27), C4(H4), C25(H25), C3(H3), C2(H2), C18(H18), C17(H17), C21(H21),
 C22(H22), C1(H1), C16(H16), C26(H26), C19(H19), C24(H24)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C15(H15A,H15B,H15C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6A)
;
_olex2_submission_special_instructions 'No special instructions were received'