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_7025309
_publ_section_title
;
 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.
;
_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            'C38 H51 Mo N3 O4'
_chemical_formula_weight         709.76
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.327(3)
_cell_length_b                   10.457(2)
_cell_length_c                   25.688(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4001.0(16)
_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 0.781
_diffrn_measured_fraction_theta_max 0.781
_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  0.1118
_diffrn_reflns_av_sigmaI/netI    0.1217
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9524
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.198
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR program, Higashi, 1995'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1001P)^2^+0.9314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.1977
_reflns_number_gt                4510
_reflns_number_total             5511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926864b.txt
_cod_data_source_block           YLWMO4
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4000.9(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7025309