Synthesis and characterization of two novel bimetallic macrocyclic complexes generated from 1,2,4-triazole-containing semi-rigid ligands and <i>M</i>(NO~3~)~2~ units (<i>M</i> = Ni and Zn)
Wu, Xiang-Wen; Yin, Shi; Wu, Wan-Fu; Ma, Jian-Ping; Acta Crystallographica Section C 72 (2016) 285–290; doi:10.1107/S205322961600348X

data_2020435
_publ_section_title
;
 Synthesis and characterization of two novel bimetallic macrocyclic
 complexes generated from 1,2,4-triazole-containing semi-rigid ligands and
 <i>M</i>(NO~3~)~2~ units (<i>M</i> = Ni and Zn)
;
_journal_coeditor_code           FM3038
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              285
_journal_page_last               290
_journal_paper_doi               10.1107/S205322961600348X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Zn2 (N O3)2 (C17 H14 N6 S)2 (C H4 O)2] (N O3)2'
_chemical_formula_moiety         'C36 H36 N14 O8 S2 Zn2 2+, 2(N O3 -)'
_chemical_formula_sum            'C36 H36 N16 O14 S2 Zn2'
_chemical_formula_weight         1111.67
_chemical_name_systematic
;Bis{\m-3-[(pyridin-4-ylmethyl)sulfanyl]-5-(quinolin-2-yl)-4<i>H</i>-1,2,4-triazol-4-amine}bis[(methanol-\k<i>O</i>)(nitrato-\k^2^<i>O</i>,<i>O</i>')
zinc(II)] dinitrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                88.257(4)
_cell_angle_beta                 81.614(4)
_cell_angle_gamma                80.184(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0414(5)
_cell_length_b                   14.4893(7)
_cell_length_c                   15.6001(8)
_cell_measurement_reflns_used    6413
_cell_measurement_temperature    100.1(5)
_cell_measurement_theta_max      71.0010
_cell_measurement_theta_min      4.2100
_cell_volume                     2212.53(19)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.1(5)
_diffrn_detector_area_resol_mean 16.0793
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova Dual Source diffractometer with Eos detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14520
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         4.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 1.0000
_diffrn_standards_interval_time  1.0000
_diffrn_standards_number         15318
_exptl_absorpt_coefficient_mu    2.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.2100
_exptl_crystal_size_mid          0.0700
_exptl_crystal_size_min          0.0400
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.824
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         7875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0600P)^2^+1.4194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                6746
_reflns_number_total             7875
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fm3038sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 2020434--2020435.cif.'
_cod_database_code               2020435
_cod_database_fobs_code          2020435