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_7232866
_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         'C25 H17 Mn N7 O5'
_chemical_formula_sum            'C25 H17 Mn N7 O5'
_chemical_formula_weight         550.40
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-10-18 deposited with the CCDC.    2019-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                66.724(9)
_cell_angle_beta                 68.005(8)
_cell_angle_gamma                77.863(7)
_cell_formula_units_Z            2
_cell_length_a                   9.3365(7)
_cell_length_b                   11.9034(11)
_cell_length_c                   11.9507(11)
_cell_measurement_reflns_used    4801
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8500
_cell_measurement_theta_min      3.7370
_cell_volume                     1128.23(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.839
_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     -9.00  85.00   1.00    2.33    --   11.74  37.00 -30.00   94
  2  \w    -10.00  38.00   1.00    2.33    --   11.74  37.00  90.00   48
  3  \w    -15.00  28.00   1.00    2.33    --  -11.59 -99.00 120.00   43
  4  \w    -65.00  30.00   1.00    2.33    --   11.74 -19.00 150.00   95
  5  \w     39.00  98.00   1.00    2.33    --   11.74-178.00-180.00   59
;
_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      -0.0175698000
_diffrn_orient_matrix_UB_12      -0.0435504000
_diffrn_orient_matrix_UB_13      0.0634975000
_diffrn_orient_matrix_UB_21      0.0236251000
_diffrn_orient_matrix_UB_22      0.0398289000
_diffrn_orient_matrix_UB_23      0.0199616000
_diffrn_orient_matrix_UB_31      -0.0766966000
_diffrn_orient_matrix_UB_32      0.0273381000
_diffrn_orient_matrix_UB_33      0.0153463000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10282
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.506
_diffrn_reflns_theta_min         3.525
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80324
_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            pink
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       block
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.9070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4590
_reflns_number_total             5286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03082d2.cif
_cod_data_source_block           0721-01
_cod_original_cell_volume        1128.2(2)
_cod_database_code               7232866
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.893
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C3(H3), C18(H18), C16(H16), C1(H1), C10(H10), C00V(H00V), C23(H23),
 C9(H9), C15(H15), C4(H4), C6(H6), C13(H13), C5(H5), C14(H14)
;
_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 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.741