Oxidation of Ni3(dpa)4Cl2 and Cu3(dpa)4Cl2: Nickel-Nickel Bonding Interaction, but No Copper-Copper Bonds
John F. Berry; F. Albert Cotton; Lee M. Daniels; Carlos A. Murillo; Xiaoping Wang; Inorganic Chemistry 42 (2003) 2418–2427; doi:10.1021/ic0262740

data_4313442
_publ_section_title
;
 Oxidation of Ni3(dpa)4Cl2 and Cu3(dpa)4Cl2: Nickel-Nickel Bonding
 Interaction, but No Copper-Copper Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2418
_journal_page_last               2427
_journal_paper_doi               10.1021/ic0262740
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        synthesis
_chemical_formula_moiety         '[Ni3(N3C10H8)4Cl2][O(C2H5)2]'
_chemical_formula_sum            'C44 H42 Cl2 N12 Ni3 O'
_chemical_formula_weight         1001.93
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.365(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9531(11)
_cell_length_b                   15.7795(8)
_cell_length_c                   17.1082(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.6
_cell_measurement_theta_min      18.2
_cell_volume                     4271.1(4)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius FAST'
_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  0.0817
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23053
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.486
_exptl_absorpt_correction_T_max  .643
_exptl_absorpt_correction_T_min  .466
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .31
_exptl_crystal_size_min          .3
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.124
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_obs          0.0808
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+30.3186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2296
_refine_ls_wR_factor_obs         0.2028
_reflns_number_observed          5869
_reflns_number_total             7478
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0262740si20030129_021710_2.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+30.3186P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+30.3186P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313442