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_4319768
_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 Mo2 N12, C7 H8'
_chemical_formula_structural     Mo2(C17H14N3)4.C7H8
_chemical_formula_sum            'C75 H64 Mo2 N12'
_chemical_formula_weight         1325.26
_chemical_name_systematic
; 
 ? 
;
_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                 106.149(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.601(2)
_cell_length_b                   32.432(2)
_cell_length_c                   18.809(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     6211.6(18)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_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       '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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24817
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         2.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.135
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         8348
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.164
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_obs          0.0485
_refine_ls_shift/esd_max         -0.056
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1384
_refine_ls_wR_factor_obs         0.1202
_reflns_number_observed          7154
_reflns_number_total             8377
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001376g_2.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^)+(0.0580P)^2^+15.0000P] 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^)+(0.0580P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319768