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_7051036
_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            'C42 H42 N4 O6 W'
_chemical_formula_weight         882.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.467(3)
_cell_length_b                   24.756(5)
_cell_length_c                   11.723(2)
_cell_measurement_reflns_used    IP
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3848.5(14)
_computing_cell_refinement       BIOTEX
_computing_data_collection       BIOTEX
_computing_data_reduction        BIOTEX
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXT
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       RAX-IIC
_diffrn_measurement_method       IP
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6301
_diffrn_reflns_theta_max         25.58
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    3.054
_exptl_absorpt_correction_T_max  1.114
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   SEMI-EMPIRICAL
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00000(5)
_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   1.058
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6301
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_obs          0.0531
_refine_ls_shift/esd_max         -0.019
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1639
_refine_ls_wR_factor_obs         0.1487
_reflns_number_observed          5295
_reflns_number_total             6301
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006979p.txt
_cod_data_source_block           '[WO2(L4)2]'
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] 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        3848.5(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7051036