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_4313445
_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         Cu3(C10H8N3)4Cl2SbCl6(C2H4Cl2)2.86(C6H12)0.792
_chemical_formula_sum            'C48.33 H48.67 Cl11.58 Cu3 N12 Sb'
_chemical_formula_weight         1520.54
_chemical_name_common            Cu3(dpa)4Cl2SbCl6(C2H4Cl2)2.86(C6H12)0.792
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   29.9365(14)
_cell_length_b                   29.9365(14)
_cell_length_c                   28.151(3)
_cell_measurement_reflns_used    7397
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.13
_cell_measurement_theta_min      4.81
_cell_volume                     25229(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55520
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.955
_exptl_absorpt_correction_T_max  0.259
_exptl_absorpt_correction_T_min  0.122
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             12120
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.333
_exptl_crystal_size_min          0.277
_refine_diff_density_max         2.706
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         9546
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+333.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1927
_reflns_number_gt                7190
_reflns_number_total             9546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0262740si20030129_021710_5.cif
_cod_data_source_block           new
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multi scan'
changed to 'multi-scan' 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_sg_symbol_H-M      'I 1 4/m 1'
_cod_database_code               4313445