μ~3~-Methoxido-κ^3^<i>O</i>:<i>O</i>:<i>O</i>-tris(μ-<small>L</small>-<i>p</i>-tyrosinato-κ^3^<i>N</i>,<i>O</i>:<i>O</i>)tris(<small>L</small>-<i>p</i>-tyrosinato-κ^2^<i>N</i>,<i>O</i>)trinickel(II,III) methanol tetrasolvate
Tapala, Weerinradah; Prior, Timothy J.; Rujiwatra, Apinpus; Acta Crystallographica Section E 69 (2013) m286–m287; doi:10.1107/S1600536813010696

data_2238058
_publ_section_title
;
 \m~3~-Methoxido-\k^3^<i>O</i>:<i>O</i>:<i>O</i>-tris(\m-<small>L</small>-<i>p</i>-tyrosinato-\k^3^<i>N</i>,<i>O</i>:<i>O</i>)tris(<small>L</small>-<i>p</i>-tyrosinato-\k^2^<i>N</i>,<i>O</i>)trinickel(II,III)
 methanol tetrasolvate
;
_journal_coeditor_code           TK5221
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m286
_journal_page_last               m287
_journal_paper_doi               10.1107/S1600536813010696
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni3 (C9 H10 N O3)6 (C H3 O)], 4C H4 O'
_chemical_formula_moiety         'C55 H63 N6 Ni3 O19, 4(C O)'
_chemical_formula_sum            'C59 H63 N6 Ni3 O23'
_chemical_formula_weight         1400.28
_chemical_name_systematic
'\m~3~-Methoxido-\k^3^<i>O</i>:<i>O</i>:<i>O</i>-tris(\m-<i>L</i>-<i>p</i>-tyrosinato-\k^3^<i>N</i>,<i>O</i>:<i>O</i>)tris(<i>L</i>-<i>p</i>-tyrosinato-\k^2^<i>N</i>,<i>O</i>)trinickel(II,III) methanol tetrasolvate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.740(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5688(6)
_cell_length_b                   25.3381(9)
_cell_length_c                   13.1058(7)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      1.55
_cell_volume                     4145.0(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS2'
_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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41350
_diffrn_reflns_theta_full        26.14
_diffrn_reflns_theta_max         26.14
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.7803
_exptl_absorpt_correction_T_min  0.7161
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(a face-indexed absorption correction was applied using the
Tompa method; Meulenaer de & Tompa, 1965)
;
_exptl_crystal_colour            light-blue
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1454
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.378
_refine_ls_abs_structure_details 'Flack (1983), 8080 Friedel pairs'
_refine_ls_abs_structure_Flack   0.023(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         16565
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                11845
_reflns_number_total             16565
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5221.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2238058
_cod_database_fobs_code          2238058