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_4106404
_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         'C39 H74 N2 P2 Si1 Ti1'
_chemical_formula_sum            'C39 H74 N2 P2 Si Ti'
_chemical_formula_weight         708.96
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-07-19
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 95.339(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.422(5)
_cell_length_b                   31.628(14)
_cell_length_c                   12.113(5)
_cell_measurement_reflns_used    2342
_cell_measurement_temperature    150
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     4357(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14982
_diffrn_reflns_theta_full        25.121
_diffrn_reflns_theta_max         25.121
_diffrn_reflns_theta_min         1.288
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9579
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3858
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.1114064
_refine_ls_shift/su_mean         0.0009708
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +10.99P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1707
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1707
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              37
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                2548
_reflns_number_total             3858
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.56
_oxford_diffrn_Wilson_scale      81.80
_oxford_refine_ls_r_factor_ref   0.1050
_oxford_refine_ls_scale          0.10991(7)
_oxford_reflns_number_all        3858
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_10074_0m in C2/c'
_cod_data_source_file            ja202316m_si_001.cif
_cod_data_source_block           10074
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C39 H74 N2 P2 Si1 Ti1'
_cod_database_code               4106404