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_7027503
_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            'C36 H30 F6 Mo N6 O6 S2'
_chemical_formula_weight         916.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 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                 97.967(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8743(12)
_cell_length_b                   10.7534(5)
_cell_length_c                   19.5999(6)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      10.79
_cell_volume                     3939.7(3)
_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      293(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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3366
_diffrn_reflns_theta_max         63.99
_diffrn_reflns_theta_min         4.56
_diffrn_standards_decay_%        5.28
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.431
_exptl_absorpt_correction_T_max  0.2056
_exptl_absorpt_correction_T_min  0.1000
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       Prisms
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       0.00123(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         3317
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.033
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_obs          0.0456
_refine_ls_shift/esd_max         -0.021
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+2.4771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1179
_refine_ls_wR_factor_obs         0.1128
_reflns_number_observed          3009
_reflns_number_total             3332
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903372fsup1.cif
_cod_data_source_block           VG9611
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0708P)^2^+2.4771P] 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^)+(0.0708P)^2^+2.4771P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Ia
_cod_original_formula_sum        'C36 H30 N6 O6 F6 S2 Mo'
_cod_database_code               7027503