Room Temperature Dehydrogenation of Ethane, Propane, Linear Alkanes C4-C8, and Some Cyclic Alkanes by Titanium-Carbon Multiple Bonds
Marco G. Crestani; Anne K. Hickey; Xinfeng Gao; Balazs Pinter; Vincent N. Cavaliere; Jun-Ichi Ito; Chun-Hsing Chen; Daniel J. Mindiola; Journal of the American Chemical Society 135 (2013) 14754–14767; doi:10.1021/ja4060178

data_4120878
_publ_section_title
;
 Room Temperature Dehydrogenation of Ethane, Propane, Linear Alkanes
 C4-C8, and Some Cyclic Alkanes by Titanium-Carbon Multiple Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14754
_journal_page_last               14767
_journal_paper_doi               10.1021/ja4060178
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C56 H88 N2 O P4 Ti2, 2 (C2 H12)'
_chemical_formula_sum            'C66 H112 N2 O P4 Ti2'
_chemical_formula_weight         1169.26
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.050(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.338(3)
_cell_length_b                   18.091(3)
_cell_length_c                   24.184(4)
_cell_measurement_reflns_used    3247
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.35
_cell_volume                     6685(2)
_computing_cell_refinement       'APEX II v2009.5.0 (Bruker, 2010)'
_computing_data_collection       'APEX II v2009.5.0 (Bruker, 2010)'
_computing_data_reduction        'APEX II v2009.5.0 (Bruker, 2010)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
'0.30 degree frames measured for 40 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  0.1759
_diffrn_reflns_av_sigmaI/netI    0.1941
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44836
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9635
_exptl_absorpt_correction_T_min  0.9288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7720
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      0.800
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0388P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                3100
_reflns_number_total             7720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4060178_si_002.cif
_cod_data_source_block           11002
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        6684.7(19)
_cod_database_code               4120878