Efficient synthesis and characterization of the low dimensional heteronuclear complexes with a N2O2-donor Schiff base ligand
Guo-Bi Li; Xu-Jia Hong; Zhi-Gang Gu; Zhi-Peng Zheng; Yang-Yang Wu; Hong-Yang Jia; Jie Liu; Yue-Peng Cai; Inorganica Chimica Acta 392 (2012) 177–183; doi:10.1016/j.ica.2012.05.031

data_1512476
_publ_section_title
;
 Efficient synthesis and characterization of the low dimensional
 heteronuclear complexes with a N2O2-donor Schiff base ligand
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              177
_journal_page_last               183
_journal_paper_doi               10.1016/j.ica.2012.05.031
_journal_volume                  392
_journal_year                    2012
_chemical_formula_sum            'C12 H19 N2 Ni O2.5'
_chemical_formula_weight         290.00
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.582(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.3332(9)
_cell_length_b                   8.4153(3)
_cell_length_c                   18.0526(11)
_cell_measurement_reflns_used    4400
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.30
_cell_measurement_theta_min      2.30
_cell_volume                     2688.7(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16268
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_T_max  0.8130
_exptl_absorpt_correction_T_min  0.7423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3094
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.6225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                2450
_reflns_number_total             3094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-177-183-1.cif
_cod_data_source_block           c
_cod_depositor_comments
;

2019-05-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C24 H38 N4 Ni2 O5'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     580.00
_cod_database_code               1512476