Crystal structures of mixed-ligand oxocyano complexes of molybdenum(IV) and tungsten(IV) and their reactivity towards molecular oxygen studied by IR spectroscopy
Dariusz Matoga; Janusz Szklarzewicz; Alina Samotus; Krzysztof Lewiński; J. Chem. Soc., Dalton Trans.  (2002) 3587–3592; doi:10.1039/b202654f

data_7011672
_publ_section_title
;
 Crystal structures of mixed-ligand oxocyano complexes of
 molybdenum(IV) and tungsten(IV) and their reactivity towards molecular
 oxygen studied by IR spectroscopy
;
_journal_issue                   18
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3587
_journal_page_last               3592
_journal_paper_doi               10.1039/b202654f
_journal_year                    2002
_chemical_formula_moiety         'C56 H50 N6 O4 P2 W'
_chemical_formula_sum            'C56 H50 N6 O4 P2 W'
_chemical_formula_weight         1116.81
_chemical_name_systematic
; 
? 
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.2620(5)
_cell_angle_beta                 89.2020(5)
_cell_angle_gamma                61.8950(5)
_cell_formula_units_Z            2
_cell_length_a                   13.6050(2)
_cell_length_b                   13.68400(10)
_cell_length_c                   16.8940(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2549.61(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans with the \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19887
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    2.380
_exptl_absorpt_correction_T_max  0.7166
_exptl_absorpt_correction_T_min  0.5354
_exptl_absorpt_correction_type
'multi-scan (DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0015(2)
_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_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         11621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.5040P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                10291
_reflns_number_total             11621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202654f.txt
_cod_data_source_block           wpz2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.5040P] 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^)+(0.0303P)^2^+1.5040P] 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               7011672