Water Displacement by Cyanogold Complexes in Binuclear Nickel(II) Compounds Based on Bridging Oxalate. Synthesis, Structural Diversity, Magnetic Properties, and DFT Calculations
Pablo Vitoria; Iñaki Muga; Juan M. Gutiérrez-Zorrilla; Antonio Luque; Pascual Román; Luis Lezama; F. Javier Zúniga; Javier I. Beitia; Inorganic Chemistry 42 (2003) 960–969; doi:10.1021/ic0203217

data_4313079
_publ_section_title
;
 Water Displacement by Cyanogold Complexes in Binuclear Nickel(II)
 Compounds Based on Bridging Oxalate. Synthesis, Structural Diversity,
 Magnetic Properties, and DFT Calculations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              960
_journal_page_last               969
_journal_paper_doi               10.1021/ic0203217
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Br2, C10 H30 Ni2 O6'
_chemical_formula_sum            'C10 H30 Br2 N6 Ni2 O6'
_chemical_formula_weight         607.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-04-02T18:59:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.546(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7178(16)
_cell_length_b                   7.3028(15)
_cell_length_c                   13.296(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.1
_cell_measurement_theta_min      6.3
_cell_measurement_wavelength     0.71073
_cell_volume                     1033.9(4)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
   x-axis points to radiation source
   the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.09323
_diffrn_orient_matrix_UB_12      -0.12899E-1
_diffrn_orient_matrix_UB_13      -0.15097E-1
_diffrn_orient_matrix_UB_21      0.4259E-2
_diffrn_orient_matrix_UB_22      -0.121981
_diffrn_orient_matrix_UB_23      0.34494E-1
_diffrn_orient_matrix_UB_31      -0.11334E-1
_diffrn_orient_matrix_UB_32      0.61152E-1
_diffrn_orient_matrix_UB_33      0.06577
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.1152
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2988
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.91
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        16
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.723
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
         Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.15
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.12
_reflns_number_gt                1642
_reflns_number_total             2988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203217_1.cif
_cod_data_source_block           comp1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4313079
_exptl_absorpt_factor_mur        1.145
_diffrn_standards_decay_corr_max 1.274
_diffrn_standards_decay_corr_min 1