Cd(ii) and Cu(ii) coordination polymers constructed from the expanded 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene ligand: conventional and ultrasound-assisted synthesis, crystal structure, luminescence and magnetic properties
Rad-Yousefnia, Negar; Shaabani, Behrouz; Zahedi, Mansoureh; Kubicki, Maciej; Aygün, Muhittin; Lloret, Francesc; Julve, Miguel; Grześkiewicz, Anita M.; Zakerhamidi, Mohammad Sadegh; Kazak, Canan; New Journal of Chemistry 42 (2018) 15860–; doi:10.1039/C8NJ02605J

data_7057660
_publ_section_title
;
 Cd(ii) and Cu(ii) coordination polymers constructed from the expanded
 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene ligand: conventional and
 ultrasound-assisted synthesis, crystal structure, luminescence and
 magnetic properties
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15860
_journal_paper_doi               10.1039/C8NJ02605J
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C12 H10 Cu N6 O6, C H Cl3'
_chemical_formula_sum            'C13 H11 Cl3 Cu N6 O6'
_chemical_formula_weight         517.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-29 deposited with the CCDC.
2018-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.285(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5429(4)
_cell_length_b                   11.9046(6)
_cell_length_c                   17.3544(10)
_cell_measurement_reflns_used    2141
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0490
_cell_measurement_theta_min      3.9250
_cell_volume                     1959.69(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_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    -26.00  77.00   1.00   45.26    --   20.07  19.00 -60.00  103
  2  \w    -10.00  55.00   1.00   45.26    --   20.07 -99.00  90.00   65
  3  \w    -17.00   9.00   1.00   45.26    --  -22.02 -99.00-150.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0185301000
_diffrn_orient_matrix_UB_12      -0.0569691000
_diffrn_orient_matrix_UB_13      0.0052638000
_diffrn_orient_matrix_UB_21      -0.0136601000
_diffrn_orient_matrix_UB_22      -0.0067450000
_diffrn_orient_matrix_UB_23      -0.0407328000
_diffrn_orient_matrix_UB_31      0.0711684000
_diffrn_orient_matrix_UB_32      -0.0160990000
_diffrn_orient_matrix_UB_33      -0.0017071000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6347
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.081
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       prism
_exptl_crystal_F_000             1036
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0440P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2712
_reflns_number_total             3944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02605j2.cif
_cod_data_source_block           iran_a425_2
_cod_depositor_comments
'Adding full bibliography for 7057660--7057662.cif.'
_cod_original_cell_volume        1959.68(17)
_cod_database_code               7057660
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C13 H11 Cl3 Cu N6 O6'
_reflns_odcompleteness_completeness 98.67
_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.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C4(H4), C1AA(H1AA), C2AA(H2AA), C7(H7), C8(H8), C9(H9), C11(H11),
 C12(H12), C13(H13)
;
_olex2_date_sample_data_collection 2015-10-16
_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 1.058
_oxdiff_exptl_absorpt_empirical_full_min 0.953