Di- and Trinuclear Complexes with the Mono- and Dianion of 2,6-Bis(phenylamino)pyridine: High-Field Displacement of Chemical Shifts Due to the Magnetic Anisotropy of Quadruple Bonds
F. Albert Cotton; Lee M. Daniels; Peng Lei; Carlos A. Murillo; Xiaoping Wang; Inorganic Chemistry 40 (2001) 2778–2784; doi:10.1021/ic001376g

data_4319767
_publ_section_title
;
 Di- and Trinuclear Complexes with the Mono- and Dianion of
 2,6-Bis(phenylamino)pyridine: High-Field Displacement of Chemical Shifts
 Due to the Magnetic Anisotropy of Quadruple Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2778
_journal_page_last               2784
_journal_paper_doi               10.1021/ic001376g
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C68 H56 Cr2 N12, C7 H8'
_chemical_formula_structural     Cr2(C17H14N3)4.C7H8
_chemical_formula_sum            'C75 H64 Cr2 N12'
_chemical_formula_weight         1237.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.94(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4601(11)
_cell_length_b                   32.321(37)
_cell_length_c                   18.7981(14)
_cell_measurement_reflns_used    248
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.
_cell_measurement_theta_min      9.1
_cell_volume                     6111(7)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'SHELXTL V5.02 (Siemens, 1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24885
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.20
_diffrn_standards_number         'None (area detector data)'
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.145
_refine_ls_goodness_of_fit_obs   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         7891
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.165
_refine_ls_restrained_S_obs      1.129
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_obs          0.0608
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1550
_refine_ls_wR_factor_obs         0.1357
_reflns_number_observed          6576
_reflns_number_total             7919
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001376g_1.cif
_cod_data_source_block           str2998
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+16.0000P] 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^)+(0.0450P)^2^+16.0000P] 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        6110.8(70)
_cod_database_code               4319767