A half-salamo-based pyridine-containing ligand and its novel Ni^II^ complexes including different auxiliary ligands: syntheses, structures, fluorescence properties, DFT calculations and Hirshfeld surface analysis
Feng, Tao; Li, Li-Li; Li, Ya-Juan; Dong, Wen-Kui; Acta Crystallographica Section B 77 (2021) 168–181; doi:10.1107/S2052520620016157

data_2108769
_publ_section_title
;
 A half-salamo-based pyridine-containing ligand and its novel Ni^II^
 complexes including different auxiliary ligands: syntheses, structures,
 fluorescence properties, DFT calculations and Hirshfeld surface analysis
;
_journal_coeditor_code           RA5088
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              168
_journal_page_last               181
_journal_paper_doi               10.1107/S2052520620016157
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Ni2 (C16 H16 N3 O4)2 (N3)2]'
_chemical_formula_moiety         'C32 H32 N12 Ni2 O8'
_chemical_formula_sum            'C32 H32 N12 Ni2 O8'
_chemical_formula_weight         830.11
_chemical_name_systematic
Bis{\m-2-methoxy-6-[8-(pyridin-2-yl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl]phenolato}bis[azidonickel(II)]
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.348(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6387(4)
_cell_length_b                   10.0171(4)
_cell_length_c                   14.7940(6)
_cell_measurement_reflns_used    5276
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.31
_cell_measurement_theta_min      5.12
_cell_volume                     1714.20(11)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL2018 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10646
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.336
_diffrn_reflns_theta_min         5.120
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2016)'
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.655
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0570
_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^)+(0.1022P)^2^+1.4134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2893
_reflns_number_total             3441
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {37ba157d-c795-4209-966f-263fed5f13da}
_cod_data_source_file            ra5088sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2108768--2108770.cif.'
_cod_database_code               2108769
_cod_database_fobs_code          2108769
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C8(H8a,H8b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C13(H13), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c)
;
_shelx_res_checksum              30037
_shelx_hkl_checksum              42394
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'