Room Temperature Dehydrogenation of Ethane to Ethylene
Vincent N. Cavaliere; Marco G. Crestani; Balazs Pinter; Maren Pink; Chun-Hsing Chen; Mu-Hyun Baik; Daniel J. Mindiola; Journal of the American Chemical Society 133 (2011) 10700–10703; doi:10.1021/ja202316m

data_4106405
_publ_section_title
;
 Room Temperature Dehydrogenation of Ethane to Ethylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10700
_journal_page_last               10703
_journal_paper_doi               10.1021/ja202316m
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C41 H66 N2 P2 Ti, 0.5 C4 H10 O'
_chemical_formula_sum            'C43 H71 N2 O0.5 P2 Ti'
_chemical_formula_weight         733.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.599(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.204(2)
_cell_length_b                   12.406(2)
_cell_length_c                   25.237(5)
_cell_measurement_reflns_used    1728
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.52
_cell_measurement_theta_min      3.64
_cell_volume                     4356.3(13)
_computing_cell_refinement       'APEX II v2009.5.0 (Bruker, 2009)'
_computing_data_collection       'APEX II v2009.5.0 (Bruker, 2009)'
_computing_data_reduction        'APEX II v2009.5.0 (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
'0.30 degree frames measured for 150 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.1494
_diffrn_reflns_av_sigmaI/netI    0.1369
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30051
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  0.9940
_exptl_absorpt_correction_T_min  0.9620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       plate
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         8249
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0478P)^2^+1.8093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                4551
_reflns_number_total             8249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja202316m_si_002.cif
_cod_data_source_block           10082
_cod_original_cell_volume        4356.4(13)
_cod_original_sg_symbol_Hall     '-P 2ybc'
_cod_original_formula_sum        'C43 H71 N2 O0.50 P2 Ti'
_cod_database_code               4106405