Synthesis and molecular structure of oxydiacetate complexes of nickel(II) and cobalt(II). Theoretical analysis of the planar and non-planar conformations of oxydiacetate ligand and oxydiacetic acid
Abdessamad Grirrane; Antonio Pastor; Andrea Ienco; Carlo Mealli; Agustín Galindo; J. Chem. Soc., Dalton Trans.  (2002) 3771–3777; doi:10.1039/b201885c

data_7011583
_publ_section_title
;
 Synthesis and molecular structure of oxydiacetate complexes of
 nickel(II) and cobalt(II). Theoretical analysis of the planar and
 non-planar conformations of oxydiacetate ligand and oxydiacetic acid
;
_journal_issue                   19
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3771
_journal_page_last               3777
_journal_paper_doi               10.1039/b201885c
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H38 N4 Ni2 O17'
_chemical_formula_structural     'C28 H38 N6 O17 NI2'
_chemical_formula_sum            'C14 H19 N2 Ni O8.5'
_chemical_formula_weight         410.02
_chemical_name_common            Ni(oda)(bipy)(H2O).1.5H2O
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-02-12T16:29:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            16
_cell_length_a                   13.560(5)
_cell_length_b                   47.533(5)
_cell_length_c                   10.781(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_measurement_wavelength     0.71073
_cell_volume                     6949(4)
_computing_cell_refinement       'Nonious CAD4 programs'
_computing_data_collection       'Nonious CAD4 programs'
_computing_data_reduction        'local routines'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'shelxl-97 (sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Nonius Cad4'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3100
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  2h
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2862
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+8.4850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                2684
_reflns_number_total             2862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201885c.txt
_cod_data_source_block           nickel
_cod_original_formula_sum        'C14 H19 N2 Ni O8.50'
_cod_database_code               7011583