Di-μ~2~-acetato-di-μ~2~-azido-di-μ~3~-methanol-tetrakis{μ-2-[(2-methyl-1-oxidopropan-2-yl)iminomethyl]-6-methoxyphenolato}tetranickel(II) methanol disolvate
Tan, Shan-Yong; Chang, Fei; Gao, Yan-Peng; Acta Crystallographica Section E 68 (2012) m150–m151; doi:10.1107/S1600536811055164

data_2233541
_publ_section_title
;
 Di-\m~2~-acetato-di-\m~2~-azido-di-\m~3~-methanol-tetrakis{\m-2-[(2-methyl-1-oxidopropan-2-yl)iminomethyl]-6-methoxyphenolato}tetranickel(II)
 methanol disolvate
;
_journal_coeditor_code           KP2370
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m150
_journal_page_last               m151
_journal_paper_doi               10.1107/S1600536811055164
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety
'[Ni4 (C12 H15 N O3)2 (C2 H3 O2)2 (N3)2 (C H4 O)2], 2(C H4 O)'
_chemical_formula_sum            'C32 H52 N8 Ni4 O14'
_chemical_formula_weight         1007.56
_chemical_name_systematic
;
Di-\m~2~-acetato-di-\m~2~-azido-di-\m~3~-methanol-tetrakis{\m-2-[(2-methyl-1-
oxidopropan-2-yl)iminomethyl]-6-methoxyphenolato}tetranickel(II)
methanol disolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.581(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5635(14)
_cell_length_b                   11.8971(16)
_cell_length_c                   18.845(3)
_cell_measurement_reflns_used    8404
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.74
_cell_volume                     2137.3(5)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15395
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.805
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1044.0
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.473
_refine_diff_density_min         -0.548
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0832P)^2^+2.6493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                4584
_reflns_number_total             5277
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            kp2370.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2233541
_cod_database_fobs_code          2233541