Bis{(<i>E</i>)-2-ethoxy-6-[2-(ethylammonio)ethyliminomethyl]phenolato}nickel(II) bis(perchlorate)
Zhu, Xue-Wen; Yang, Xu-Zhao; Acta Crystallographica Section E 64 (2008) m1096–m1097; doi:10.1107/S1600536808023684

data_2219175
_publ_section_title
;Bis{(<i>E</i>)-2-ethoxy-6-[2-(ethylammonio)ethyliminomethyl]phenolato}nickel(II)
 bis(perchlorate)
;
_journal_coeditor_code           SJ2526
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1096
_journal_page_last               m1097
_journal_paper_doi               10.1107/S1600536808023684
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C13 H20 N2 O2)2] (Cl O4)2'
_chemical_formula_moiety         'C26 H40 N4 Ni O4 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C26 H40 Cl2 N4 Ni O12'
_chemical_formula_weight         730.23
_chemical_name_systematic
;Bis{(<i>E</i>)-2-Ethoxy-6-[2-(ethylammonio)ethyliminomethyl]phenolato}nickel(II)
bis(perchlorate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.068(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.386(3)
_cell_length_b                   8.566(3)
_cell_length_c                   21.862(6)
_cell_measurement_reflns_used    3252
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.5
_cell_volume                     1550.8(9)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w 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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12509
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.8458
_exptl_absorpt_correction_T_min  0.8256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.343
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.4599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                2770
_reflns_number_total             3363
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2526.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2219175
_cod_database_fobs_code          2219175