New dioxo-molybdenum(VI) and -tungsten(VI) complexes with N-capped tripodal N₂O₂ tetradentate ligands: synthesis, structures and catalytic activities towards olefin epoxidation.
Wong, Yee-Lok; Tong, Lok H.; Dilworth, Jonathan R.; Ng, Dennis K. P.; Lee, Hung Kay; Dalton transactions (Cambridge, England : 2003) 39 (2010) 4602–4611; doi:10.1039/b926864b

data_7025308
_publ_section_title
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 New dioxo-molybdenum(VI) and -tungsten(VI) complexes with N-capped
 tripodal N&#x2082;O&#x2082; tetradentate ligands: synthesis, structures
 and catalytic activities towards olefin epoxidation.
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_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4602
_journal_page_last               4611
_journal_paper_doi               10.1039/b926864b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C28 H34 N2 O4 W'
_chemical_formula_weight         646.42
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.257(4)
_cell_length_b                   12.703(3)
_cell_length_c                   20.780(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5347.2(19)
_computing_cell_refinement       'BioteX software MSC 1995'
_computing_data_collection       'RAXIS-IIC RIGAKU'
_computing_data_reduction        'BioteX software MSC 1995'
_computing_molecular_graphics    'SHELXTL Vers. 6.10 (Sheldrick, 2000)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Rigaku RAXIS-IIC imaging plate'
_diffrn_measurement_method       'phi oscillation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1555
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_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12458
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    4.356
_exptl_absorpt_correction_T_max  1.194
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR program, Higashi, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
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_refine_ls_extinction_coef       0.0025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
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_refine_ls_number_reflns         4113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.1008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1678P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2514
_reflns_number_gt                3544
_reflns_number_total             4113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926864b.txt
_cod_data_source_block           YLWW01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7025308