Remarkable Effects of Axial π* Coordination on the Cr-Cr Quadruple Bond in Dichromium Paddlewheel Complexes
F. Albert Cotton; Lee M. Daniels; Carlos A. Murillo; Isabel Pascual; Hong-Cai Zhou; Journal of the American Chemical Society 121 (1999) 6856–6861; doi:10.1021/ja9912675

data_4116453
_publ_section_title
;
 Remarkable Effects of Axial \p* Coordination on the Cr-Cr Quadruple Bond
 in Dichromium Paddlewheel Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6856
_journal_page_last               6861
_journal_paper_doi               10.1021/ja9912675
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_moiety         'Cr2 (C17 H16 N3)4, (C H2 Cl2)'
_chemical_formula_structural     'Cr2 (DPhIP)4, CH2Cl2'
_chemical_formula_sum            'C69 H66 Cl2 Cr2 N12'
_chemical_formula_weight         1238.24
_chemical_name_systematic
; 
 Tetrakis(2,6-diphenyliminopiperidinato)dichromium(II) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 110.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.197(3)
_cell_length_b                   16.467(8)
_cell_length_c                   29.511(10)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     12385(8)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23353
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        none
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       plate
_exptl_crystal_F_000             5168
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         7868
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.168
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_obs          0.0704
_refine_ls_shift/esd_max         -0.031
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+104.5229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1890
_refine_ls_wR_factor_obs         0.1596
_reflns_number_observed          6655
_reflns_number_total             8068
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9912675_4.cif
_cod_data_source_block           1.CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+104.5229P] 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^)+(0.0563P)^2^+104.5229P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        12385.1(72)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4116453