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_4070200
_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         'C48 H60 Cr N4 O0.50 P4 W '
_chemical_formula_sum            'C48 H60 Cr N4 O0.5 P4 W'
_chemical_formula_weight         1060.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.8723(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.0977(3)
_cell_length_b                   19.5256(6)
_cell_length_c                   21.2340(5)
_cell_measurement_reflns_used    36420
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.9
_cell_volume                     4557.8(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.119
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42313
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_exptl_absorpt_coefficient_mu    2.943
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.540
_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
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2152.00
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.33
_refine_diff_density_min         -1.99
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     581
_refine_ls_number_reflns         10339
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                6338
_reflns_number_total             10349
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om9006467_si_001.cif
_cod_data_source_block           '_4_WCr1Et'
_cod_original_formula_sum        'C48 H60 Cr N4 O0.50 P4 W '
_cod_database_code               4070200