A bicontinuous donor‒acceptor hybrid heterostructure based on coordination and cation‒π interactions
Li, Meng-Hua; You, Ming-Hua; Zhang, Jiang-Yan; Xiao, Wang-Chuan; Lin, Mei-Jin; CrystEngComm 20 (2018) 7795–; doi:10.1039/C8CE01526K

data_7231753
_publ_section_title
;
 A bicontinuous donor--acceptor hybrid heterostructure based on
 coordination and cation--\p interactions
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              7795
_journal_paper_doi               10.1039/C8CE01526K
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C16 H8 Cu2 N7 S2, C7 H4 N2 S'
_chemical_formula_sum            'C23 H12 Cu2 N9 S3'
_chemical_formula_weight         637.68
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-16 deposited with the CCDC.
2018-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                84.614(5)
_cell_angle_beta                 70.854(6)
_cell_angle_gamma                80.244(5)
_cell_formula_units_Z            2
_cell_length_a                   9.5199(7)
_cell_length_b                   10.2672(6)
_cell_length_c                   12.5352(8)
_cell_measurement_reflns_used    8532
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3000
_cell_measurement_theta_min      2.6510
_cell_volume                     1139.75(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     49.00  75.00   0.50    7.81    --    5.00   0.00  90.00   52
  2  \w    -29.00  81.00   0.50    7.81    --   -7.70  55.00 150.00  220
  3  \w    -96.00 -65.00   0.50    7.81    --   -7.70  14.00   0.00   62
  4  \w    -23.00  72.00   0.50    7.81    --   -7.70  55.00  30.00  190
  5  \w    -91.00 -65.00   0.50    7.81    --   -7.70  55.00 -90.00   52
  6  \w      3.00  74.00   0.50    7.81    --   -7.70  55.00 -90.00  142
  7  \w    -81.00 -53.00   0.50    7.81    --   -7.70  55.00  30.00   56
  8  \w    -50.00 -24.00   0.50    7.81    --   -7.70  14.00   0.00   52
  9  \w     17.00  80.00   0.50    7.81    --   -7.70  14.00   0.00  126
 10  \w    -80.00 -54.00   0.50    7.81    --   -7.70  55.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0515785000
_diffrn_orient_matrix_UB_12      -0.0583131000
_diffrn_orient_matrix_UB_13      -0.0178598000
_diffrn_orient_matrix_UB_21      -0.0062426000
_diffrn_orient_matrix_UB_22      -0.0188737000
_diffrn_orient_matrix_UB_23      0.0570852000
_diffrn_orient_matrix_UB_31      -0.0604920000
_diffrn_orient_matrix_UB_32      -0.0341375000
_diffrn_orient_matrix_UB_33      0.0040142000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15203
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.436
_refine_diff_density_min         -2.722
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4486
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0497
_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^)+(0.1041P)^2^+3.9915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                3964
_reflns_number_total             4486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce01526k2.cif
_cod_data_source_block           li8
_cod_depositor_comments          'Adding full bibliography for 7231753.cif.'
_cod_original_cell_volume        1139.75(13)
_cod_database_code               7231753
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 N006, C010
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1, C00V
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W), C00Y(H00Y), C00Z(H00Z)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.450
_oxdiff_exptl_absorpt_empirical_full_min 0.835