Unprecedented five-fold interpenetrated donor-acceptor hybrid heterostructure induced by anion-π interactions
You, Ming-Hua; Li, Meng-Hua; Liu, Yong-Fei; Li, Hao-Hong; Lin, Mei-Jin; CrystEngComm  (2019) –; doi:10.1039/C9CE01416K

data_7234566
_publ_section_title
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 Unprecedented five-fold interpenetrated donor-acceptor hybrid
 heterostructure induced by anion-\p interactions
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01416K
_journal_year                    2019
_chemical_formula_moiety         '2(C3 Fe0.5 N3), 2(C12 H7 N2 O2), C3 H7 N O'
_chemical_formula_sum            'C33 H21 Fe N11 O5'
_chemical_formula_weight         707.46
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-08-03
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.31 svn.r3643 for OlexSys, GUI svn.r5859)
;
_audit_update_record
;
2019-08-03 deposited with the CCDC.    2019-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                112.203(4)
_cell_angle_beta                 112.169(5)
_cell_angle_gamma                101.951(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8757(7)
_cell_length_b                   13.7673(6)
_cell_length_c                   13.9810(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1940.2(2)
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.834
_diffrn_measured_fraction_theta_max 0.834
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.1203
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26813
_diffrn_reflns_theta_full        29.53
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.439
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             724
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0004(10)
_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   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                4380
_reflns_number_total             9042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ce01416k2.cif
_cod_data_source_block           dpndi-fe
_cod_original_cell_volume        1940.19(16)
_cod_database_code               7234566
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N9(H9A), C26(H26), C2(H2), N2(H2A), C30(H30), C1(H1), C21(H21), C20(H20),
 C12(H12), C11(H11), C19(H19), C9(H9), C23(H23), C10(H10), C33(H33)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'