Syntheses, structures, and magnetic properties of mixed-ligand complexes based on 3,6-bis(benzimidazol-1-yl)pyridazine
Dong, Jun-Liang; Zhu, Peng-Yin; Du, Jia-Qiang; Xie, Fei; Lan, Hai-Ming; Yang, Ru-Xia; Yang, Li-Zheng; Wang, Duo-Zhi; RSC Advances 9 (2019) 17560–; doi:10.1039/C9RA03082D

data_7232864
_publ_section_title
;
 Syntheses, structures, and magnetic properties of mixed-ligand complexes
 based on 3,6-bis(benzimidazol-1-yl)pyridazine
;
_journal_issue                   31
_journal_name_full               'RSC Advances'
_journal_page_first              17560
_journal_paper_doi               10.1039/C9RA03082D
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C26 H18 N6 Ni O5'
_chemical_formula_sum            'C26 H18 N6 Ni O5'
_chemical_formula_weight         553.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-18 deposited with the CCDC.    2019-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.235(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7121(4)
_cell_length_b                   6.1520(2)
_cell_length_c                   16.1276(4)
_cell_measurement_reflns_used    6651
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.0590
_cell_measurement_theta_min      3.2790
_cell_volume                     1161.77(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.887
_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    -57.00  40.00   1.00    2.38    --   11.74 -57.00-150.00   97
  2  \w    -14.00  80.00   1.00    2.38    --   11.74  77.00 120.00   94
  3  \w    -10.00  82.00   1.00    2.38    --   11.74  57.00   0.00   92
  4  \w    -35.00  41.00   1.00    2.38    --  -11.59  57.00 120.00   76
  5  \w    -16.00  45.00   1.00    2.38    --   11.74  57.00-120.00   61
  6  \w      4.00  70.00   1.00    2.38    --   11.74-128.00  38.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0474428000
_diffrn_orient_matrix_UB_12      0.0274709000
_diffrn_orient_matrix_UB_13      -0.0245325000
_diffrn_orient_matrix_UB_21      -0.0098579000
_diffrn_orient_matrix_UB_22      0.1118273000
_diffrn_orient_matrix_UB_23      0.0078150000
_diffrn_orient_matrix_UB_31      0.0363485000
_diffrn_orient_matrix_UB_32      -0.0055983000
_diffrn_orient_matrix_UB_33      0.0356727000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14734
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.619
_diffrn_reflns_theta_min         2.127
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.418(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5313
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0218P)^2^+0.2985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                4954
_reflns_number_total             5313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03082d2.cif
_cod_data_source_block           2hao_0115
_cod_database_code               7232864
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.893
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.582(13)
 0.418(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Rotating group:
 O1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C15(H15), C2(H2), C24(H24), C22(H22), C12(H12), C17(H17), C25(H25),
 C21(H21), C16(H16), C18(H18), C3(H3), C9(H9), C10(H10), C4(H4), C5(H5)
;
_shelx_res_checksum              37957
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.694
_oxdiff_exptl_absorpt_empirical_full_min 0.763