Oxidative Scission of a Mo-Mo Quadruple Bond
F. Albert Cotton; Carlos A. Murillo; Hong-Cai Zhou; Inorganic Chemistry 39 (2000) 3261–3264; doi:10.1021/ic000092t

data_4321136
_publ_section_title
;
 Oxidative Scission of a Mo-Mo Quadruple Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3261
_journal_page_last               3264
_journal_paper_doi               10.1021/ic000092t
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Mo2 (C17 H16 N3)4 (P F6),2(C H2 Cl2)'
_chemical_formula_structural     'Mo2 (DPhIP)4 (PF6),2(CH2Cl2)'
_chemical_formula_sum            'C70 H68 Cl4 F6 Mo2 N12 P'
_chemical_formula_weight         1556.01
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
; 
 Tetrakis(2,6-di(phenylimino)piperidinatodimolybdenum(II,III) 
 hexafluorophosphate 
;
_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                 106.403(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1891(9)
_cell_length_b                   17.8073(10)
_cell_length_c                   24.210(2)
_cell_measurement_reflns_used    242
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.83
_cell_volume                     7108.9(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 system'
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14409
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         'none (area detector data set)'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3172
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    'not treated (disordered)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         4584
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.089
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_obs          0.0862
_refine_ls_shift/esd_max         -0.764
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+146.3954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2343
_refine_ls_wR_factor_obs         0.2069
_reflns_number_observed          3802
_reflns_number_total             4600
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000092t_2.cif
_cod_data_source_block           1.2CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+146.3954P] 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^)+(0.0895P)^2^+146.3954P] 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        7108.8(7)
_cod_database_code               4321136