Highly interlocked anion-bridged supramolecular networks from interrupted imidazole-urea gels
Samuel J. James; Andrea Perrin; Christopher D. Jones; Dmitry S. Yufit; Jonathan W. Steed; Chem.Commun. 50 (2014) 12851–; doi:10.1039/C4cc05789A

data_7115815
_publ_section_title
;
 Highly interlocked anion-bridged supramolecular networks from interrupted
 imidazole-urea gels
;
_journal_name_full               Chem.Commun.
_journal_page_first              12851
_journal_paper_doi               10.1039/C4cc05789A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C78 H96 Cu N24 O6, 2(N O3), 2(C H4 O)'
_chemical_formula_sum            'C80 H104 Cu N26 O14'
_chemical_formula_weight         1717.43
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                75.123(4)
_cell_angle_beta                 77.751(4)
_cell_angle_gamma                74.712(4)
_cell_formula_units_Z            1
_cell_length_a                   13.1000(7)
_cell_length_b                   13.3909(7)
_cell_length_c                   13.4410(6)
_cell_measurement_reflns_used    8330
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.3799
_cell_measurement_theta_min      1.5836
_cell_volume                     2171.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0435482000
_diffrn_orient_matrix_UB_12      0.0425846000
_diffrn_orient_matrix_UB_13      0.0097994000
_diffrn_orient_matrix_UB_21      0.0334869000
_diffrn_orient_matrix_UB_22      0.0213317000
_diffrn_orient_matrix_UB_23      0.0201076000
_diffrn_orient_matrix_UB_31      0.0145072000
_diffrn_orient_matrix_UB_32      0.0298359000
_diffrn_orient_matrix_UB_33      -0.0505406000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29444
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.587
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear bluish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             907
_exptl_crystal_size_max          0.3434
_exptl_crystal_size_mid          0.1879
_exptl_crystal_size_min          0.1443
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         8537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0750P)^2^+1.3369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6765
_reflns_number_total             8537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05789a2.cif
_cod_data_source_block           sj4f
_cod_original_cell_volume        2171.59(19)
_cod_database_code               7115815
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C39H48N13O6Cu
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. 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, All O(H) groups
2. Others
 Fixed Sof: O4(0.6) H4C(0.6) O8(0.4) H8B(0.4) C1A(0.6) H1AA(0.6) H1AB(0.6)
 H1AC(0.6) C1B(0.4) H1BA(0.4) H1BB(0.4) H1BC(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C4(H4A,H4B), C17(H17A,H17B), C18(H18A,H18B),
 C5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C11(H11A), C14(H14), C8(H8A), C35(H35), C27(H27), C15(H15), C34(H34),
 C38(H38), C12(H12A), C37(H37), C24(H24), C2(H2A), C25(H25), C22(H22), C9(H9),
 C28(H28), C21(H21)
3.c Idealised Me refined as rotating group:
 C13(H13B,H13C,H13A), C26(H26A,H26B,H26C), C39(H39A,H39B,H39C), C1A(H1AA,H1AB,
 H1AC), C1B(H1BA,H1BB,H1BC)
3.d Idealised tetrahedral OH refined as rotating group:
 O4(H4C), O8(H8B)
;
_shelx_res_checksum              21332
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'