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_7232865
_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         'C24 H16 Mn N6 O5 S'
_chemical_formula_sum            'C24 H16 Mn N6 O5 S'
_chemical_formula_weight         555.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-09
_audit_creation_method
;
Olex2 1.2-beta
(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                 109.388(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.829(3)
_cell_length_b                   5.8486(10)
_cell_length_c                   20.750(3)
_cell_measurement_reflns_used    2515
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.18
_cell_volume                     2270.0(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16528
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         1.040
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0960 before and 0.0606 after correction. The Ratio of minimum to maximum transmission is 0.8223. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 1857 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         4747
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.6832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4455
_reflns_number_total             4747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03082d2.cif
_cod_data_source_block           mo_201797-ycy-4_0m
_cod_database_code               7232865
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.63(2)
 0.37(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
N4A \\sim N3A \\sim C16A \\sim C15A \\sim C16 \\sim N4 \\sim N3 \\sim C15:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(N4A)=Sof(N3A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=1-FVAR(1)
 Sof(C16)=Sof(H16)=Sof(N4)=Sof(N3)=Sof(C15)=Sof(H15)=FVAR(1)
5.a Rotating group:
 O5(H5A,H5B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C20(H20), C12(H12), C22(H22), C11(H11), C9(H9), C18(H18),
 C4(H4), C23(H23), C16A(H16A), C21(H21), C15A(H15A), C10(H10), C16(H16),
 C15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'