cis-Dioxo-tungsten(VI) and -molybdenum(VI) complexes with N2O2 tetradentate ligands: synthesis, structure, electrochemistry and oxo-transfer properties
Wong, Yee-Lok; Yan, Yan; Chan, Edith S. H.; Yang, Qingchuan; Mak, Thomas C. W.; Ng, Dennis K. P.; Journal of the Chemical Society, Dalton Transactions  (1998) 3057–; doi:10.1039/a804425b

data_7027915
_publ_section_title
;
 cis-Dioxo-tungsten(VI) and -molybdenum(VI) complexes with N2O2
 tetradentate ligands: synthesis, structure, electrochemistry and
 oxo-transfer properties
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3057
_journal_paper_doi               10.1039/a804425b
_journal_year                    1998
_chemical_formula_sum            'C18 H22 N2 O4 W'
_chemical_formula_weight         514.23
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 119.400(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0150(14)
_cell_length_b                   7.4238(5)
_cell_length_c                   14.8940(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1831.7(2)
_computing_cell_refinement       'BIOTEX Rigaku'
_computing_data_collection       'RAXIS Rigaku'
_computing_data_reduction        'BIOTEX Rigaku'
_computing_molecular_graphics    'Seimens SHELXTL'
_computing_publication_material  'Seimens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'IP Rigaku'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2778
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    6.331
_exptl_absorpt_correction_T_max  1.362
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.611
_refine_diff_density_min         -2.234
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.30(2)
_refine_ls_extinction_coef       0.0000(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_all   1.050
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2722
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.204
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_obs          0.0539
_refine_ls_shift/esd_max         -1.393
_refine_ls_shift/esd_mean        0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1246P)^2^+1.2537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1660
_refine_ls_wR_factor_obs         0.1453
_reflns_number_observed          2671
_reflns_number_total             2778
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b804425sup1.cif
_cod_data_source_block           d3
_cod_depositor_comments
;
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^)+(0.1246P)^2^+1.2537P] 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^)+(0.1246P)^2^+1.2537P] 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      C2
_cod_database_code               7027915