High oxidation state chromium, molybdenum and tungsten imido metallasiloxanes
King, Lawrence; Motevalli, Majid; Sullivan, Alice C.; Journal of the Chemical Society, Dalton Transactions  (1999) 3225–; doi:10.1039/a904429i

data_7027583
_publ_section_title
;
 High oxidation state chromium, molybdenum and tungsten imido
 metallasiloxanes
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3225
_journal_paper_doi               10.1039/a904429i
_journal_year                    1999
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C56 H64 N2 O4 Si4 W1'
_chemical_formula_structural     'C56 H64 O4 N2 SI4 W'
_chemical_formula_sum            'C63 H66 N2 O6 Si4 W'
_chemical_formula_weight         1243.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             1999-05-28T15:04:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                110.88(6)
_cell_angle_beta                 90.08(4)
_cell_angle_gamma                99.91(4)
_cell_formula_units_Z            1
_cell_length_a                   10.333(4)
_cell_length_b                   10.733(8)
_cell_length_c                   14.149(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1440.9(15)
_computing_cell_refinement       'CAD4/PC (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4/PC (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.71874E-1
_diffrn_orient_matrix_UB_12      -0.26556E-1
_diffrn_orient_matrix_UB_13      -0.04606
_diffrn_orient_matrix_UB_21      -0.67239E-1
_diffrn_orient_matrix_UB_22      -0.50682E-1
_diffrn_orient_matrix_UB_23      -0.57802E-1
_diffrn_orient_matrix_UB_31      0.4106E-2
_diffrn_orient_matrix_UB_32      0.08405
_diffrn_orient_matrix_UB_33      -0.16236E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5351
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.14
_exptl_absorpt_correction_T_max  0.6394
_exptl_absorpt_correction_T_min  0.4091
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            'COLOURLESS, TRANSPARENT'
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.059
_refine_diff_density_min         -6.047
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.208
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                4787
_reflns_number_total             5054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904429Isup1.cif
_cod_data_source_block           wdiol
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-08-02
;
_cod_original_cell_volume        1440.9(14)
_cod_original_sg_symbol_Hall     P-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027583
_exptl_absorpt_factor_mur        0.443
_exptl_absorpt_correction_t_ave  0.5529
_diffrn_standards_decay_corr_max 1.08
_diffrn_standards_decay_corr_min 0.997