Synthesis and structures of dioxo-Mo(VI) and -W(VI) amides
Kay Lee, Hung; Wong, Yee-Lok; Zhou, Zhong-Yuan; Zhang, Ze-Ying; Ng, Dennis K. P.; Mak, Thomas C. W.; Journal of the Chemical Society, Dalton Transactions  (2000) 539–; doi:10.1039/a907811h

data_7008999
_publ_section_title
;
 Synthesis and structures of dioxo-Mo(VI) and -W(VI) amides
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              539
_journal_paper_doi               10.1039/a907811h
_journal_year                    2000
_chemical_formula_sum            'C24 H42 Mo N4 O2 Si2'
_chemical_formula_weight         570.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.342(3)
_cell_length_b                   16.007(3)
_cell_length_c                   22.218(4)
_cell_measurement_temperature    294(2)
_cell_volume                     5811.9(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.681
_diffrn_measured_fraction_theta_max 0.681
_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    0.1064
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3746
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.8774
_exptl_absorpt_correction_T_min  0.8239
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0007(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_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         3746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.2051
_reflns_number_gt                3050
_reflns_number_total             3746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907811h.txt
_cod_data_source_block           yl2
_cod_original_cell_volume        5812(2)
_cod_database_code               7008999