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_7009001
_publ_section_title
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 Synthesis and structures of dioxo-Mo(VI) and -W(VI) amides
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_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            'C18 H30 Mo N4 O2 Si2'
_chemical_formula_weight         486.58
_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                 97.38(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.931(3)
_cell_length_b                   11.888(2)
_cell_length_c                   14.295(3)
_cell_measurement_reflns_used    IP
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     2347.8(8)
_computing_cell_refinement       BIOTEX
_computing_data_collection       BIOTEX
_computing_data_reduction        BIOTEX
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7569
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  1.068
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            golden
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0122(7)
_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   1.095
_refine_ls_goodness_of_fit_obs   1.099
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_obs          0.0372
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+0.6492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1390
_refine_ls_wR_factor_obs         0.1364
_reflns_number_observed          4074
_reflns_number_total             4261
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a907811h.txt
_cod_data_source_block           lhk15
_cod_depositor_comments
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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^)+(0.0738P)^2^+0.6492P] 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^)+(0.0738P)^2^+0.6492P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009001