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_4313443
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, PO Box  30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_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_formula_moiety         'Ni6 C114 H110 N24 Cl4'
_chemical_formula_sum            'C114 H110 Cl4 N24 Ni6'
_chemical_formula_weight         2310.32
_chemical_name_common            '[Ni3(dpa)4Cl2]2*4toluene*hexane'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.277(5)
_cell_angle_beta                 81.847(8)
_cell_angle_gamma                63.449(6)
_cell_formula_units_Z            2
_cell_length_a                   16.991(2)
_cell_length_b                   18.211(2)
_cell_length_c                   19.138(3)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.6
_cell_measurement_theta_min      18.2
_cell_volume                     5206.3(12)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  '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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27153
_diffrn_reflns_theta_full        22.59
_diffrn_reflns_theta_max         22.59
_diffrn_reflns_theta_min         2.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  1.22
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark putple'
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         13178
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.575
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+18.2557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                11252
_reflns_number_total             13178
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0262740si20030129_021710_3.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'not measured' 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        5206.4(12)
_cod_database_code               4313443