Synthesis, structure and oxo-transfer properties of dioxotungsten(VI) complexes with pyridine-based NO-and NS-bidentate ligands
Wong, Yee-Lok; Yang, Qingchuan; Zhou, Zhong-Yuan; Kay Lee, Hung; Mak, Thomas C. W.; Ng, Dennis K. P.; New Journal of Chemistry 25 (2001) 353–; doi:10.1039/b006979p

data_7051037
_publ_section_title
;
 Synthesis, structure and oxo-transfer properties of dioxotungsten(VI)
 complexes with pyridine-based NO-and NS-bidentate ligands
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              353
_journal_paper_doi               10.1039/b006979p
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C53.5 H63.5 N2.5 O4.5 W'
_chemical_formula_weight         997.42
_chemical_name_systematic
;
 ?
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.760(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.660(3)
_cell_length_b                   16.118(1)
_cell_length_c                   19.974(3)
_cell_measurement_temperature    294(2)
_cell_volume                     5444.0(13)
_computing_cell_refinement       'BIOTEX Rigaku'
_computing_data_collection       'RAXIS Rigaku'
_computing_data_reduction        'BIOTEX Rigaku'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.712
_diffrn_measured_fraction_theta_max 0.712
_diffrn_measurement_device_type  '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    0.1138
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7249
_diffrn_reflns_theta_full        25.55
_diffrn_reflns_theta_max         25.55
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_T_max  1.118
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   abscor
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.00015(4)
_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   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7249
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.133
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.1951
_reflns_number_gt                5316
_reflns_number_total             7249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006979p.txt
_cod_data_source_block           '[WO2(L5)2]'
_cod_original_cell_volume        5444(1)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C53.50 H63.50 N2.50 O4.50 W'
_cod_database_code               7051037