Selective and Effective Stabilization of MoVI=O Bonds by NH...S Hydrogen Bonds via Trans Influence
Taka-aki Okamura; Miki Tatsumi; Yui Omi; Hitoshi Yamamoto; Kiyotaka Onitsuka; Inorganic Chemistry 51 (2012) 11688–11697; doi:10.1021/ic301597d

data_4330886
_publ_section_title
;
 Selective and Effective Stabilization of MoVI=O Bonds by NH...S Hydrogen
 Bonds via Trans Influence
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11688
_journal_page_last               11697
_journal_paper_doi               10.1021/ic301597d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C21 H31 N O3 S2'
_chemical_formula_sum            'C21 H31 N O3 S2'
_chemical_formula_weight         409.59
_chemical_name_systematic
; 
1,2-(t-BuCOS)2-3-t-BuNHCOC6H3 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             'Wed Aug 18 20:31:44 2004'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.75(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.384(18)
_cell_length_b                   10.493(15)
_cell_length_c                   19.37(2)
_cell_measurement_reflns_used    14011
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     2309(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22080
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                3163
_reflns_number_total             5277
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301597d_si_002_2.cif
_cod_data_source_block           2,3-(t-BuCOS)2C6H3CONH-t-Bu
_cod_original_cell_volume        2309(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4330886