Syntheses, Structures, and DFT Calculations of Phosphenium Phosphite Complexes of Molybdenum: Preference of Nonbridging Form to Bridging Form of a Donor Group
Nakazawa, Hiroshi; Miyoshi, Yasutaka; Katayama, Takafumi; Mizuta, Tsutomu; Miyoshi, Katsuhiko; Tsuchida, Noriko; Ono, Ayako; Takano, Keiko; Organometallics 25 (2006) 5913–; doi:10.1021/om060639x

data_4074435
_publ_section_title
;
 Syntheses, Structures, and DFT Calculations of Phosphenium Phosphite
 Complexes of Molybdenum:&#x00A0; Preference of Nonbridging Form to
 Bridging Form of a Donor Group
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5913
_journal_paper_doi               10.1021/om060639x
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C18 H39 Mo N6 O6 P3'
_chemical_formula_sum            'C18 H39 Mo N6 O6 P3'
_chemical_formula_weight         624.40
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.694(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.703(3)
_cell_length_b                   17.963(3)
_cell_length_c                   9.744(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      15.1
_cell_volume                     2890.0(9)
_computing_cell_refinement       'MXC system'
_computing_data_collection       'MXC system'
_computing_data_reduction        'MXC system'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'MacScience MXC3 kappa'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    5.2398
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8680
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.68
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0047(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         8096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.5743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                6714
_reflns_number_total             8096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060639xsi20060714_013713.cif
_cod_data_source_block           miyoshi1
_cod_original_cell_volume        2890.0(10)
_cod_database_code               4074435