Linear Connection of Four Nitrile Molecules on the Tetraphosphine Complexes of Tungsten and Molybdenum
Dai, Qi Xiu; Seino, Hidetake; Mizobe, Yasushi; Organometallics  (2014) 140702100106004–; doi:10.1021/om500405f

data_4083866
_publ_section_title
;
 Linear Connection of Four Nitrile Molecules on the Tetraphosphine
 Complexes of Tungsten and Molybdenum
;
_journal_name_full               Organometallics
_journal_page_first              140702100106004
_journal_paper_doi               10.1021/om500405f
_journal_year                    2014
_chemical_formula_moiety         'C89 H62 F24 Mo N4 P4'
_chemical_formula_sum            'C89 H62 F24 Mo N4 P4'
_chemical_formula_weight         1863.29
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.4221(17)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.744(5)
_cell_length_b                   24.892(8)
_cell_length_c                   22.143(7)
_cell_measurement_reflns_used    11016
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      3.04
_cell_volume                     8119(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50459
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3768.00
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.540
_refine_diff_density_min         -1.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         15559
_refine_ls_number_restraints     54
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1292P)^2^+18.0598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2482
_reflns_number_gt                10175
_reflns_number_total             15564
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500405f_si_002.cif
_cod_data_source_block           '_[Mo(NCArF)4(P4)]'
_cod_database_code               4083866