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_4083865
_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         'C54 H54 Mo P4'
_chemical_formula_sum            'C54 H54 Mo P4'
_chemical_formula_weight         922.86
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                75.083(8)
_cell_angle_beta                 69.027(8)
_cell_angle_gamma                68.883(8)
_cell_formula_units_Z            2
_cell_length_a                   11.8801(16)
_cell_length_b                   13.2558(17)
_cell_length_c                   16.210(2)
_cell_measurement_reflns_used    6294
_cell_measurement_temperature    113
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.66
_cell_volume                     2199.2(5)
_computing_cell_refinement       TwinSolve
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        TwinSolve
_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 7.353
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.165
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17025
_diffrn_reflns_theta_full        27.30
_diffrn_reflns_theta_max         27.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             960.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.990
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     695
_refine_ls_number_reflns         17025
_refine_ls_number_restraints     3
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0440P)^2^+10.3525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1778
_reflns_number_gt                12714
_reflns_number_total             17025
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500405f_si_002.cif
_cod_data_source_block           '[Mo(cod)(P4)]_twin'
_cod_original_cell_volume        2199.2(6)
_cod_database_code               4083865
_twin_formation_mechanism        gt
_twin_dimensionality             triperiodic
_twin_morphology                 contact