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_4319770
_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         'C100 H132 Cr3 N14, C8 H8 O2'
_chemical_formula_structural     '[Bu4N]2[Cr3(bpap)4] 2THF'
_chemical_formula_sum            'C108 H140 Cr3 N14 O2'
_chemical_formula_weight         1822.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 123.385(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.483(6)
_cell_length_b                   14.080(2)
_cell_length_c                   26.842(4)
_cell_measurement_reflns_used    951
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.74
_cell_volume                     9935(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'XP (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       'Bruker SMART'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27427
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.169
_refine_ls_goodness_of_fit_obs   1.235
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_restrained_S_obs      1.235
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_obs          0.0764
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2162
_refine_ls_wR_factor_obs         0.1873
_reflns_number_observed          6367
_reflns_number_total             9220
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001376g_4.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+25.0000P] 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^)+(0.0800P)^2^+25.0000P] 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        9934.7(30)
_cod_database_code               4319770