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_4330885
_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         'C38 H66 Mo N4 O3 S4'
_chemical_formula_sum            'C38 H66 Mo N4 O3 S4'
_chemical_formula_weight         851.13
_chemical_name_systematic
; 
(NEt4)2[MoO(S2C6H3CONH-t-Bu)2] 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-08-25
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8717(17)
_cell_length_b                   16.213(4)
_cell_length_c                   30.046(5)
_cell_measurement_reflns_used    27375
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.06
_cell_volume                     4321.7(15)
_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 R-AXIS RAPID'
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            34363
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9484
_exptl_absorpt_correction_T_min  0.8778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7615
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0506P)^2^+22.2822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1696
_reflns_number_gt                6915
_reflns_number_total             7615
_reflns_threshold_expression     I>\2s(I)
_cod_data_source_file            ic301597d_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        4321.8(14)
_cod_database_code               4330885