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_4313441
_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)4Cl2 SbCl6 (C3H6O)2.44'
_chemical_formula_sum            'C47.31 H46.63 Cl8 Cu3 N12 O2.44 Sb'
_chemical_formula_weight         1418.31
_chemical_name_common            'Cu3(dpa)4Cl2SbCl6 2.44(acetone)'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.506(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0331(12)
_cell_length_b                   12.4010(10)
_cell_length_c                   33.114(3)
_cell_measurement_radiation      CuK\a
_cell_measurement_reflns_used    11979
_cell_measurement_temperature    173
_cell_measurement_theta_max      59.56
_cell_measurement_theta_min      2.68
_cell_measurement_wavelength     1.54051
_cell_volume                     6088.5(9)
_computing_cell_refinement       TwinSolve
_computing_data_collection       CrystalClear
_computing_data_reduction        TwinSolve
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_type            'R-AXIS-CS3 6.X, c++'
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_details      '600 images in steps of   1.000\%'
_diffrn_measurement_device_details 'Curved image plate'
_diffrn_measurement_device_type  'R-AXIS-CS3 6.X, c++'
_diffrn_measurement_method       'profile data'
_diffrn_measurement_specimen_support 'glass fiber'
_diffrn_orient_matrix_type
;  x  =  h UB
   coordinate system: 
     x from crystal towards source
     z vertical, towards goniometer base
     y so that x,y,z is right-handed
;
_diffrn_orient_matrix_UB_11      0.005159
_diffrn_orient_matrix_UB_12      0.023372
_diffrn_orient_matrix_UB_13      0.063071
_diffrn_orient_matrix_UB_21      0.058571
_diffrn_orient_matrix_UB_22      0.050267
_diffrn_orient_matrix_UB_23      -0.023418
_diffrn_orient_matrix_UB_31      -0.020238
_diffrn_orient_matrix_UB_32      0.022936
_diffrn_orient_matrix_UB_33      -0.001385
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_polarisn_norm  0.00
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            57715
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        54.24
_diffrn_reflns_theta_max         54.24
_diffrn_reflns_theta_min         11.16
_diffrn_source_current           40
_diffrn_source_power             2.0
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    8.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  Shape and scale corrections using equivalent reflections.
   Shape function based on spherical harmonics.
   Highest even and odd order for spherical harmonics:  4  and  1
   Laue group:  2/m (b)
   Friedel opposites are equivalent.

_exptl_absorpt_correction_T_min            0.3404
_exptl_absorpt_correction_T_max            1.0000

_exptl_absorpt_correction_T_min            0.4419
_exptl_absorpt_correction_T_max            1.0000

_exptl_absorpt_correction_T_min            0.5201
_exptl_absorpt_correction_T_max            1.0000

;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             2832
_exptl_crystals_number           1
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         57875
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.1087
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+140.7733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2416
_reflns_number_gt                44705
_reflns_number_total             57875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0262740si20030129_021710_1.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 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_database_code               4313441