Syntheses, structures, electrochemical and optical properties of four transition metal complexes based on the 1-triazolyl-3-benzimidazolyltriazene ligand
Qiu, Yan-Xuan; Miao, Yu; Wang, Zi-Zhou; Li, Zhi-Xin; Ouyang, Zhi-Jian; Yang, Liu; Lin, Wen-Ning; Feng, Wei-Jin; Dong, Wen; RSC Adv.  (2016) –; doi:10.1039/C5RA21057G

data_7223747
_publ_section_title
;
 Syntheses, structures, electrochemical and optical properties of four
 transition metal complexes based on the
 1-triazolyl-3-benzimidazolyltriazene ligand
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA21057G
_journal_year                    2016
_chemical_formula_moiety         'C40 H40 N36 Ni3, C3 O, O2, 2(O)'
_chemical_formula_sum            'C43 H40 N36 Ni3 O5'
_chemical_formula_weight         1317.18
_chemical_name_systematic        'Nickel complex'
_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
_audit_creation_date             2015-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-29 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.480(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7945(11)
_cell_length_b                   15.2176(14)
_cell_length_c                   19.0428(18)
_cell_measurement_reflns_used    4165
_cell_measurement_temperature    296(2)
_cell_volume                     3293.9(5)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26830
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.983
_diffrn_reflns_theta_min         1.738
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7519
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0654
_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^)+(0.1190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.2130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3864
_reflns_number_total             7938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra21057g2.cif
_cod_data_source_block           1
_cod_database_code               7223747
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 C22-C21
 1.4 with sigma of 0.02
3. Rigid bond restraints
 O1, C22, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C21 \\sim C22 \\sim C23: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O1W) \\sim Ueq, Uanis(O1X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O1(0.5) C21(0.5) C22(0.5) C23(0.5) O1W(0.5) O1X(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N17(H17A,H17B), N18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 N7(H7), N10(H10), C1(H1), C5(H5), C6(H6), C7(H7A), C8(H8), C12(H12), C13(H13),
  C14(H14), C15(H15), C18(H18)
;
_shelx_res_checksum              12015
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id 1
_olex2_submission_special_instructions 'No special instructions were received'