Preparation and Protonation of Tungsten- and Molybdenum-Dinitrogen Complexes Bearing Bis(dialkylphosphinobenzene)chromiums as Auxiliary Ligands
Yuki, Masahiro; Miyake, Yoshihiro; Nishibayashi, Yoshiaki; Organometallics 28 (2009) 5821–; doi:10.1021/om9006467

data_4070201
_publ_section_title
;
 Preparation and Protonation of Tungsten- and Molybdenum-Dinitrogen
 Complexes Bearing Bis(dialkylphosphinobenzene)chromiums as Auxiliary
 Ligands
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5821
_journal_paper_doi               10.1021/om9006467
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C40 H60 Cr2 Mo N4 O2 P4 '
_chemical_formula_sum            'C40 H60 Cr2 Mo N4 O2 P4'
_chemical_formula_weight         952.77
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.5417(3)
_cell_length_b                   10.0118(3)
_cell_length_c                   28.9647(6)
_cell_measurement_reflns_used    28305
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     4216.93(18)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_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'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            38509
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1976.00
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4787
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.5500\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                3326
_reflns_number_total             4787
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om9006467_si_001.cif
_cod_data_source_block           '_5_MoCr2Me'
_cod_original_cell_volume        4216.91(18)
_cod_original_formula_sum        'C40 H60 Cr2 Mo N4 O2 P4 '
_cod_database_code               4070201