μ-Acetato-μ-(5-chloro-2-{1,3-bis[2-(5-chloro-2-oxidobenzylideneamino)ethyl]imidazolidin-2-yl}phenolato)-bis[methanolnickel(II)] methanol monosolvate monohydrate
Khan, Ahmed Raza; Tesema, Yohannes; Butcher, Ray J.; Gultneh, Yilma; Acta Crystallographica Section E 67 (2011) m1264–m1265; doi:10.1107/S1600536811032727

data_2231577
_publ_section_title
;
 \m-Acetato-\m-(5-chloro-2-{1,3-bis[2-(5-chloro-2-oxidobenzylideneamino)ethyl]imidazolidin-2-yl}phenolato)-bis[methanolnickel(II)]
 methanol monosolvate monohydrate
;
_journal_coeditor_code           JJ2099
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1264
_journal_page_last               m1265
_journal_paper_doi               10.1107/S1600536811032727
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Ni2 (C2 H3 O2) (C H4 O)2 (C27 H24 Cl3 N4 O3)], C H4 O, H2 O'
_chemical_formula_moiety         'C31 H35 Cl3 N4 Ni2 O7, C H4 O, H2 O'
_chemical_formula_sum            'C32 H41 Cl3 N4 Ni2 O9'
_chemical_formula_weight         849.46
_chemical_name_systematic
;
\m-Acetato-\m-(\m-5-chloro-2-{1,3-bis[2-(5-chloro-
2-oxidobenzylideneamino)ethyl]imidazolidin-2-yl}phenolato)-
bis[methanolnickel(II)] methanol monosolvate monohydrate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.684(2)
_cell_length_b                   16.042(2)
_cell_length_c                   13.7868(19)
_cell_measurement_reflns_used    4340
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.054
_cell_measurement_theta_min      2.294
_cell_volume                     3690.0(8)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       '\f and \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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23326
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.226
_refine_ls_abs_structure_details 'Flack (1983), no. of Friedel pairs?'
_refine_ls_abs_structure_Flack   0.017(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8737
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                7189
_reflns_number_total             8737
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jj2099.cif
_cod_data_source_block           I
_cod_original_cell_volume        3690.1(9)
_cod_database_code               2231577
_cod_database_fobs_code          2231577