Syntheses and Structures of Isoindoline Complexes of Zn(II) and Cu(II): An Unexpected Trinuclear Zn(II) Complex
Oren P. Anderson; Agnete la Cour; Andrew Dodd; Andrew D. Garrett; Mark Wicholas; Inorganic Chemistry 42 (2003) 122–127; doi:10.1021/ic011246n

data_4312844
_publ_section_title
;
 Syntheses and Structures of Isoindoline Complexes of Zn(II) and Cu(II):
 An Unexpected Trinuclear Zn(II) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              122
_journal_page_last               127
_journal_paper_doi               10.1021/ic011246n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C20 H20 Cl Cu N5 O6'
_chemical_formula_weight         525.40
_chemical_name_common
;
[Cu(4'-MeL)(H2O2)2]ClO4; 4'-MeLH =
1,3-bis{2-(4-methylpyridyl)imino}isoindoline
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            8
_cell_length_a                   17.663(3)
_cell_length_b                   14.223(2)
_cell_length_c                   16.925(3)
_cell_measurement_temperature    154(2)
_cell_volume                     4251.9(12)
_computing_cell_refinement       'SMART, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      154(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS SMART CCD area detector'
_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  0.0990
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34950
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0070(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0545P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                3212
_reflns_number_total             4698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011246n_1.cif
_cod_data_source_block           sadmw4_Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4251.9(13)
_cod_database_code               4312844