Formation of Ammonia in the Reactions of a Tungsten Dinitrogen with Ruthenium Dihydrogen Complexes under Mild Reaction Conditions1
Yoshiaki Nishibayashi; Shin Takemoto; Shotaro Iwai; Masanobu Hidai; Inorganic Chemistry 39 (2000) 5946–5957; doi:10.1021/ic000799f

data_4321708
_publ_section_title
;
 Formation of Ammonia in the Reactions of a Tungsten Dinitrogen with
 Ruthenium Dihydrogen Complexes under Mild Reaction Conditions1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5946
_journal_page_last               5957
_journal_paper_doi               10.1021/ic000799f
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C36 H50 F6 N2 O6.5 P4 S2 W'
_chemical_formula_weight         1100.66
_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'
_audit_creation_date             'Fri Feb  4 21:16:03 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 109.24(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.818(5)
_cell_length_b                   33.978(6)
_cell_length_c                   12.163(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.5
_cell_volume                     4611(3)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.05761
_diffrn_orient_matrix_UB_12      0.00530
_diffrn_orient_matrix_UB_13      -0.07966
_diffrn_orient_matrix_UB_21      0.00412
_diffrn_orient_matrix_UB_22      -0.02829
_diffrn_orient_matrix_UB_23      -0.02105
_diffrn_orient_matrix_UB_31      -0.06853
_diffrn_orient_matrix_UB_32      -0.00615
_diffrn_orient_matrix_UB_33      0.02818
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.078
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8507
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        -22.94
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.805
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2208.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.96
_refine_diff_density_min         -1.14
_refine_ls_extinction_coef       0.00177(10)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.678
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     504
_refine_ls_number_reflns         5395
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.0580
_refine_ls_shift/su_mean         0.0080
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0331
_reflns_number_gt                5395
_reflns_number_total             8097
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic000799f.cif
_cod_data_source_block           19(THF)0.5
_cod_original_cell_volume        4611(2)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C36 H50 F6 N2 O6.50 P4 S2 W '
_cod_database_code               4321708