High oxidation state imido metallasiloxanes: synthesis and structural characterisation of novel bis-imido chromium(VI) and molybdenum(VI) compounds †
King, Lawrence; Motevalli, Majid; Sullivan, Alice C.; Journal of the Chemical Society, Dalton Transactions  (2000) 1357–; doi:10.1039/a909712k

data_7009278
_publ_section_title
;
 High oxidation state imido metallasiloxanes: synthesis and structural
 characterisation of novel bis-imido chromium(VI) and molybdenum(VI)
 compounds&#x200A;&#x2020;
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1357
_journal_paper_doi               10.1039/a909712k
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H40 Cl2 Mo1 N4'
_chemical_formula_structural     'C40 H40 N4 CL2 MO'
_chemical_formula_sum            'C37.5 H47.5 Cl2 Mo N4'
_chemical_formula_weight         721.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1999-11-11T16:39:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.62(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.689(6)
_cell_length_b                   37.658(8)
_cell_length_c                   10.246(4)
_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                     3720(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (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-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_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      0.82042E-1
_diffrn_orient_matrix_UB_12      0.3539E-2
_diffrn_orient_matrix_UB_13      -0.50579E-1
_diffrn_orient_matrix_UB_21      -0.35936E-1
_diffrn_orient_matrix_UB_22      0.23908E-1
_diffrn_orient_matrix_UB_23      -0.28847E-1
_diffrn_orient_matrix_UB_31      0.51919E-1
_diffrn_orient_matrix_UB_32      0.11132E-1
_diffrn_orient_matrix_UB_33      0.79488E-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    0.0851
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6378
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        7
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.8831
_exptl_absorpt_correction_T_min  0.7066
_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            orange
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1506
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.245
_refine_diff_density_min         -3.886
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.914
_refine_ls_goodness_of_fit_gt    1.036
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_restrained_S_obs      1.036
_refine_ls_R_factor_all          0.1639
_refine_ls_R_factor_gt           0.1067
_refine_ls_shift/su_max          -0.106
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3358
_refine_ls_wR_factor_gt          0.2893
_reflns_number_gt                3822
_reflns_number_total             6378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909712k.txt
_cod_data_source_block           moar1
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-08-02

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+50.0000P] 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^)+(0.2000P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3721(3)
_cod_original_sg_symbol_Hall     '-P 2yac'
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C37.50 H47.50 Cl2 Mo N4'
_cod_database_code               7009278
_exptl_absorpt_factor_mur        0.123
_exptl_absorpt_correction_t_ave  0.7987
_diffrn_standards_decay_corr_max 1.368
_diffrn_standards_decay_corr_min 0.95