Unexpected CC Bond Formation via Doubly Dehydrogenative Coupling of Two Saturated sp3 C-H Bonds Activated with a Polymolybdate
Qiang Li; Yongge Wei; Jian Hao; Yulin Zhu; Longsheng Wang; Journal of the American Chemical Society 129 (2007) 5810–5811; doi:10.1021/ja070600z

data_4109384
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
P. R. China
;
_publ_contact_author_email       ygwei@pku.edu.cn
_publ_contact_author_name        'Dr Yongge Wei'
_publ_section_title
;
 Unexpected CC Bond Formation via Doubly Dehydrogenative Coupling of Two
 Saturated sp3 C-H Bonds Activated with a Polymolybdate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5810
_journal_page_last               5811
_journal_paper_doi               10.1021/ja070600z
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C36.5 H79 Mo6 N3 O18'
_chemical_formula_weight         1423.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.39(3)
_cell_angle_beta                 89.96(3)
_cell_angle_gamma                80.54(3)
_cell_formula_units_Z            2
_cell_length_a                   11.875(2)
_cell_length_b                   12.894(3)
_cell_length_c                   18.939(4)
_cell_measurement_reflns_used    19713
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.00
_cell_volume                     2777.9(11)
_computing_cell_refinement       'Rigaku RAPID AUTO Ver2.30'
_computing_data_collection       'Rigaku RAPID AUTO Ver2.30'
_computing_data_reduction        'Rigaku RAPID AUTO Ver2.30'
_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      293(2)
_diffrn_detector_area_resol_mean '100x100 micron'
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       Oscillation
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17074
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.6830
_exptl_absorpt_correction_T_min  0.6091
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             1430
_exptl_crystal_size_max          0.40
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_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         8990
_refine_ls_number_restraints     623
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1313
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0893P)^2^+1.8531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1871
_reflns_number_gt                4485
_reflns_number_total             8990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070600zsi20070131_093632.cif
_cod_data_source_block           Mo12-Hex-Pr-Compound-9
_cod_original_cell_volume        2778.1(10)
_cod_original_formula_sum        'C36.50 H79 Mo6 N3 O18'
_cod_database_code               4109384