Divergent reactivity of nitric oxide with metal-metal quintuple bonds
Pei-Fang Wu; Shih-Cheng Liu; Yun-Jen Shieh; Ting-Shen Kuo; Gene-Hsiang Lee; Yu Wang; Yi-Chou Tsai; Chem.Commun. 49 (2013) 4391–; doi:10.1039/c3cc37118b

data_7109245
_publ_section_title
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 Divergent reactivity of nitric oxide with metal-metal quintuple bonds
;
_journal_name_full               Chem.Commun.
_journal_page_first              4391
_journal_paper_doi               10.1039/c3cc37118b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C62 H78 Mo2 N6 O4', 0.7(C6 H14)'
_chemical_formula_sum            'C66.2 H87.8 Mo2 N6 O4'
_chemical_formula_weight         1223.50
_chemical_name_systematic
;
?
;
_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                 99.118(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5514(13)
_cell_length_b                   13.6186(13)
_cell_length_c                   34.248(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     6240.6(10)
_computing_cell_refinement       'Bruker APEX II'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            40388
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.9393
_exptl_absorpt_correction_T_min  0.8053
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2572
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
The unit cell volume comprises a large region of disordered solvent which could not be modeled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 137.6 electrons per unit cell, which were assigned to be 2.8 n-hexane molecules per unit cell.
;
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+4.4411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                8751
_reflns_number_total             10905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc37118b.txt
_cod_data_source_block           a10393
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C66.20 H87.80 Mo2 N6 O4'
_cod_database_code               7109245