Semiconductive coordination polymers with continuous π-π interactions and defined crystal structures.
Yan, Yong; Henfling, Stefan; Zhang, Ning-Ning; Krautscheid, Harald; Chemical communications (Cambridge, England) 57 (2021) 10407–10410; doi:10.1039/d1cc03333f

data_7128959
_publ_section_title
;
 Semiconductive coordination polymers with continuous \p-\p interactions
 and defined crystal structures.
;
_journal_issue                   80
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10407
_journal_page_last               10410
_journal_paper_doi               10.1039/d1cc03333f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'C18 H15 N3 O7'
_chemical_formula_weight         385.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-09-01 deposited with the CCDC.	2021-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                78.791(4)
_cell_angle_beta                 82.589(4)
_cell_angle_gamma                67.238(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4711(3)
_cell_length_b                   8.7536(4)
_cell_length_c                   14.0801(7)
_cell_measurement_reflns_used    7989
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      70.55
_cell_measurement_theta_min      5.55
_cell_volume                     831.44(7)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29437
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.974
_diffrn_reflns_theta_min         5.551
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_correction_T_min  0.2494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMA, Acetonitril'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0759
_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^)+(0.1315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2285
_refine_ls_wR_factor_ref         0.2537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2778
_reflns_number_total             5795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03333f2.cif
_cod_data_source_block           h2ondi
_cod_depositor_comments
'Adding full bibliography for 7128957--7128960.cif.'
_cod_database_code               7128959
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.980
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.724(2)
 0.276(2)
2. 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
3.a Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C9(H9)
3.c Idealised tetrahedral OH refined as rotating group:
 O002(H002), O005(H005)
;
_shelx_res_checksum              10089
_shelx_hkl_checksum              72750