Dichloro(1,2-dimethoxyethane)bis(tosylimido)molybdenum(VI), a versatile nitrene transfer reagent
Rufanov, Konstantin A.; Ziemer, Burkhard; Acta Crystallographica Section C 62 (2006) m54–m55; doi:10.1107/S0108270105042484

data_2014417
_publ_section_title
;
 Dichloro(1,2-dimethoxyethane)bis(tosylimido)molybdenum(VI), a
 versatile nitrene transfer reagent
;
_journal_coeditor_code           TY1010
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m54
_journal_page_last               m55
_journal_paper_doi               10.1107/S0108270105042484
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mo (C7 H7 N O2 S)2 Cl2 (C4 H10 O2)]'
_chemical_formula_moiety         'C18 H24 Cl2 Mo N2 O6 S2'
_chemical_formula_sum            'C18 H24 Cl2 Mo N2 O6 S2'
_chemical_formula_weight         595.35
_chemical_melting_point          431.0(10)
_chemical_name_common
;
Dichloro(1,2-dimethoxyethane)bis(tosylimido)molybdenum(VI)
;
_chemical_name_systematic
;
Dichloro(dimethoxyethano)bis(para-toluenesulfonimino-N)molybdenum(VI)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.66(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.895(2)
_cell_length_b                   13.124(2)
_cell_length_c                   15.564(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2350.6(7)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1997)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method
'\f oscillation scans, increment 1.2\%, 200 exposures'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15274
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.8564
_exptl_absorpt_correction_T_min  0.5853
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
[ABSCOR (Higashi, 1995), a modification of DIFABS (Walker & Stuart,
1983).
In contrast with DIFABS, ABSCOR loads F^2^ values instead of F values.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.673
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0437P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                3598
_reflns_number_total             4329
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ty1010.cif
_cod_data_source_block           I
_cod_original_cell_volume        2350.7(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2014417
_cod_database_fobs_code          2014417