Intramolecular "Aryl-Metal Chelate Ring" π,π-Interactions as Structural Evidence for Metalloaromaticity in (Aromatic α,α'-Diimine)-Copper(II) Chelates: Molecular and Crystal Structure of Aqua(1,10-phenanthroline)(2-benzylmalonato)copper(II) Three-hydrate
A. Castiñeiras; A. G. Sicilia-Zafra; J. M. González-Pérez; D. Choquesillo-Lazarte; J. Niclós-Gutiérrez; Inorganic Chemistry 41 (2002) 6956–6958; doi:10.1021/ic026004h

data_4319090
_publ_section_title
;
 Intramolecular "Aryl-Metal Chelate Ring" \p,\p-Interactions as Structural
 Evidence for Metalloaromaticity in (Aromatic \a,\a'-Diimine)-Copper(II)
 Chelates: Molecular and Crystal Structure of
 Aqua(1,10-phenanthroline)(2-benzylmalonato)copper(II) Three-hydrate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6956
_journal_page_last               6958
_journal_paper_doi               10.1021/ic026004h
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C22 H24 Cu N2 O8'
_chemical_formula_weight         507.97
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.964(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2142(6)
_cell_length_b                   13.4539(14)
_cell_length_c                   18.738(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      13.793
_cell_measurement_theta_min      7.041
_cell_volume                     2263.7(4)
_computing_cell_refinement       'CAD4-Express Software (Nonius, 1994)'
_computing_data_collection       'CAD4-Express Software (Nonius, 1994)'
_computing_data_reduction        'GENHKL (Kretschmar, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       omega-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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6977
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.9053
_exptl_absorpt_correction_T_min  0.6307
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            sky-blue
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0572P)^2^+0.7940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                3959
_reflns_number_total             5464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026004h-2_s1.cif
_cod_data_source_block           01tjn03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

'_symmetry_cell_setting' value 'Monoclinic'
changed to 'monoclinic' 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 
;
_cod_original_cell_volume        2263.6(4)
_cod_database_code               4319090