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_7027584
_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_formula_structural     'C64 H76 O6 SI2 N2 MO'
_chemical_formula_sum            'C62 H59 Mo N3 O6 Si4'
_chemical_formula_weight         1150.42
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             1999-05-14T15:44:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.67(8)
_cell_angle_beta                 87.75(6)
_cell_angle_gamma                107.62(6)
_cell_formula_units_Z            2
_cell_length_a                   13.655(9)
_cell_length_b                   14.524(10)
_cell_length_c                   16.072(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      8.5
_cell_measurement_wavelength     0.71073
_cell_volume                     2963(4)
_computing_cell_refinement       'CAD4 /PC (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 /PC (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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      -0.7119E-2
_diffrn_orient_matrix_UB_12      -0.72265E-1
_diffrn_orient_matrix_UB_13      -0.16325E-1
_diffrn_orient_matrix_UB_21      0.63605E-1
_diffrn_orient_matrix_UB_22      0.14404E-1
_diffrn_orient_matrix_UB_23      -0.34015E-1
_diffrn_orient_matrix_UB_31      0.42628E-1
_diffrn_orient_matrix_UB_32      0.6933E-2
_diffrn_orient_matrix_UB_33      0.51534E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.2165
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10401
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.51
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.4872
_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            'transparent yellow'
_exptl_crystal_density_diffrn    1.29
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.812
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10401
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.2446
_refine_ls_R_factor_gt           0.113
_refine_ls_shift/su_max          2.837
_refine_ls_shift/su_mean         0.095
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2557
_refine_ls_wR_factor_ref         0.3015
_reflns_number_gt                3858
_reflns_number_total             10401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904429Isup1.cif
_cod_data_source_block           motetr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               7027584
_exptl_absorpt_factor_mur        0.047
_exptl_absorpt_correction_t_ave  0.6754
_diffrn_standards_decay_corr_max 1.083
_diffrn_standards_decay_corr_min 0.991