Multiple Modes for Coordination of Phenazine to Molybdenum: Ring Fusion Promotes Access to η4-Coordination, Oxidative Addition of Dihydrogen and Hydrogenation of Aromatic Nitrogen Compounds
Sattler, Aaron; Zhu, Guang; Parkin, Gerard; Journal of the American Chemical Society 131 (2009) 7828–7838; doi:10.1021/ja901896x

data_4104505
_publ_section_title
;
 Multiple Modes for Coordination of Phenazine to Molybdenum: Ring Fusion
 Promotes Access to \h4-Coordination, Oxidative Addition of Dihydrogen and
 Hydrogenation of Aromatic Nitrogen Compounds
;
_journal_coden_ASTM              JACSAT
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7828
_journal_page_last               7838
_journal_paper_doi               10.1021/ja901896x
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C45 H88 Mo2 N2 P6'
_chemical_formula_weight         1034.87
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1740(16)
_cell_length_b                   9.4426(8)
_cell_length_c                   26.621(2)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.29
_cell_volume                     4529.5(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            71261
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_correction_T_min  0.7613
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The unit cell contains 4 pentane molecules which have been treated as a
diffuse contribution to the overall scattering without specific atom positions
by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         13827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.4743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                10288
_reflns_number_total             13827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901896x_si_004.cif
_cod_data_source_block           mo246s10p
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-09
;
_cod_original_cell_volume        4529.5(7)
_cod_database_code               4104505