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_4321135
_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 (B F4),5(C2 H3 N),(C4 H10 O)'
_chemical_formula_structural     'Mo2 (DPhIP)4 (BF4)2,5(CH3CN),(Et2O)'
_chemical_formula_sum            'C82 H89 B2 F8 Mo2 N17 O'
_chemical_formula_weight         1694.20
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Tetrakis(2,6-di(phenylimino)piperidinato)dimolybdenum(III,III) 
bis(tetrafluoroborate) 
;
_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                 93.48(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.523(5)
_cell_length_b                   27.418(5)
_cell_length_c                   18.163(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     8213(3)
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29358
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         10343
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_obs          0.0535
_refine_ls_shift/esd_max         -0.022
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+36.3676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1472
_refine_ls_wR_factor_obs         0.1310
_reflns_number_observed          9244
_reflns_number_total             10516
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000092t_1.cif
_cod_data_source_block           2.5CH3CN.Et2O
_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 'none' 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^)+(0.0561P)^2^+36.3676P] 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^)+(0.0561P)^2^+36.3676P] 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        8213.0(32)
_cod_database_code               4321135