β-Hydrogen Abstraction of an Ethyl Group Provides Entry to Titanium and Zirconium Ethylene Complexes
Kamitani, Masahiro; Searles, Keith; Chen, Chun-Hsing; Carroll, Patrick J.; Mindiola, Daniel J.; Organometallics 34 (2015) 2558–; doi:10.1021/om501226k

data_4085741
_publ_section_title
;
 \b-Hydrogen Abstraction of an Ethyl Group Provides Entry to Titanium and
 Zirconium Ethylene Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2558
_journal_paper_doi               10.1021/om501226k
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C29 H46 F3 N1 O3 P2 S1 Zr1'
_chemical_formula_sum            'C29 H46 F3 N O3 P2 S Zr'
_chemical_formula_weight         698.92
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-06-20
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.6098(4)
_cell_length_b                   26.6098(4)
_cell_length_c                   9.6169(2)
_cell_measurement_reflns_used    8766
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     6809.5(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.040
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25483
_diffrn_reflns_theta_full        26.400
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         1.082
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.91
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9719
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6918
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.0225871
_refine_ls_shift/su_mean         0.0011255
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +23.41P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1103
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1103
_reflns_limit_h_max              33
_reflns_limit_h_min              -33
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                6145
_reflns_number_total             6945
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.30
_oxford_diffrn_Wilson_scale      229.83
_oxford_refine_ls_r_factor_ref   0.0570
_oxford_refine_ls_scale          0.074751(15)
_oxford_reflns_number_all        6918
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_13081_0m in I-4'
_cod_data_source_file            om501226k_si_003.cif
_cod_data_source_block           13081
_cod_depositor_comments
'Adding full bibliography for 4085740--4085741.cif.'
_cod_original_sg_symbol_H-M      'I -4 '
_cod_original_formula_sum        'C29 H46 F3 N1 O3 P2 S1 Zr1'
_cod_database_code               4085741
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT ZR   (    1 ,X'S,U'S) 
CONT S    (    1 ,X'S,U'S)  UNTIL S    (   11 ) 
CONT P    (    1 ,X'S,U'S)  UNTIL P    (    2 ) 
CONT F    (    1 ,X'S,U'S)  UNTIL F    (   31 ) 
CONT O    (    1 ,X'S,U'S) 
CONT O    (    2 ,X'S,U'S)  UNTIL O    (   31 ) 
CONT N    (    1 ,X'S,U'S)  UNTIL C    (   28 ) 
CONT C    (   29 ,X'S,U'S)  UNTIL C    (  291 ) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) H   ( 163,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) H   ( 203,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = S(11) TO C(291) 
U(IJ)'S  0.0, 0.010000 = S(1) TO C(29) 
RESTRAIN 0.0 0.005 = C(29, U[11]) - C( 29, U[33]) 
RESTRAIN 0.0 0.005 = O(2, U[11]) - O( 2, U[22]) 
RESTRAIN 0.0 0.01 = O(2, U[13]) - O( 2, U[12]) 
U(IJ)'S  0.0, 0.005000 = F(21) TO O(2) 
U(IJ)'S  0.0, 0.005000 = F(2) TO O(31) 
U(IJ)'S  0.0, 0.005000 = F(3) TO F(31) 
U(IJ)'S  0.0, 0.010000 = F(2) TO F(3) 
U(IJ)'S  0.0, 0.010000 = F(11) TO F(31) 
END                                                                             
;