Bis(isodiazene) and related complexes of molybdenum(VI). Syntheses and structures of [Mo(OTf )2(NNPh2)2(py)2], [MoCl(OTf )(NNPh2){NC5H3(CH2C(O)Ph2)2-2,6}], [{MoCl(NNPh2)2(μ-Cl)(NH2But)}2] and [MoTp′Cl(NNPh2)2] [OTf = O3SCF3, Tp′ = tris(3,5-dimethylpyrazolyl)hydroborate]
Dilworth, Jonathan R.; Gibson, Vernon C.; Davies, Nicola; Redshaw, Carl; White, Andrew P.; Williams, David J.; Journal of the Chemical Society, Dalton Transactions  (1999) 2695–; doi:10.1039/a903372f

data_7027504
_publ_section_title
;
 Bis(isodiazene) and related complexes of molybdenum(VI). Syntheses and
 structures of [Mo(OTf&#x200A;)2(NNPh2)2(py)2],
 [MoCl(OTf&#x200A;)(NNPh2){NC5H3(CH2C(O)Ph2)2-2,6}],
 [{MoCl(NNPh2)2(\m-Cl)(NH2But)}2] and [MoTp&#x2032;Cl(NNPh2)2]
 [OTf&#x2005;=&#x2005;O3SCF3,
 Tp&#x2032;&#x2005;=&#x2005;tris(3,5-dimethylpyrazolyl)hydroborate]
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2695
_journal_paper_doi               10.1039/a903372f
_journal_year                    1999
_chemical_formula_sum            'C47.5 H40 Cl4 F3 Mo N3 O5 S'
_chemical_formula_weight         1059.63
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                119.41(2)
_cell_angle_beta                 91.321(14)
_cell_angle_gamma                95.50(2)
_cell_formula_units_Z            2
_cell_length_a                   12.900(2)
_cell_length_b                   14.588(3)
_cell_length_c                   14.795(3)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      12.35
_cell_measurement_theta_min      4.95
_cell_volume                     2406.3(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6069
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.12
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.9515
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       Prisms
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         5707
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.057
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_obs          0.0628
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.3727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1705
_refine_ls_wR_factor_obs         0.1494
_reflns_number_observed          4210
_reflns_number_total             5708
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903372fsup1.cif
_cod_data_source_block           VG9609
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.3727P] 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^)+(0.0920P)^2^+0.3727P] 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        2406.4(8)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C47.50 H40 N3 O5 F3 S Cl4 Mo'
_cod_database_code               7027504