Crystal structures and 77Se NMR spectra of molybdenum(IV) areneselenolates having intramolecular NH...Se hydrogen bonds.
Okamura, Taka-Aki; Taniuchi, Kaku; Lee, Keonil; Yamamoto, Hitoshi; Ueyama, Norikazu; Nakamura, Akira; Inorganic chemistry 45 (2006) 9374–9380; doi:10.1021/ic061140y

data_4350541
_publ_section_title
;
 Crystal structures and 77Se NMR spectra of molybdenum(IV)
 areneselenolates having intramolecular NH...Se hydrogen bonds.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9374
_journal_page_last               9380
_journal_paper_doi               10.1021/ic061140y
_journal_volume                  45
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C80 H72 N4 Mo O5 P2 Se4'
_chemical_formula_sum            'C80 H72 Mo N4 O5 P2 Se4'
_chemical_formula_weight         1643.14
_chemical_name_systematic
; 
(PPh4)2[MoO(Se-2-CH3CONHC6H4)4] 
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Fri Nov 19 09:25:03 2004'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.728(15)
_cell_length_b                   13.149(11)
_cell_length_c                   19.335(15)
_cell_measurement_reflns_used    16197
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     3527(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1272
_diffrn_reflns_av_sigmaI/netI    0.2897
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28251
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    2.351
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.329(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.644
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         11068
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.645
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                4823
_reflns_number_total             11068
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic061140ysi20060623_074848.cif
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4350541