Unsymmetrical Saturated Ketones Resulting from Activations of Hydrocarbon C(sp3)‒H and C(sp2)‒H Bonds Effected by Cp*W(NO)(H)(η3-allyl) Complexes
Baillie, Rhett A.; Lefèvre, Guillaume P.; Wakeham, Russell J.; Holmes, Aaron S.; Legzdins, Peter; Organometallics 34 (2015) 4085–; doi:10.1021/acs.organomet.5b00537

data_4087717
_publ_section_title
;
 Unsymmetrical Saturated Ketones Resulting from Activations of Hydrocarbon
 C(sp3)--H and C(sp2)--H Bonds Effected by Cp*W(NO)(H)(\h3-allyl)
 Complexes
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_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4085
_journal_paper_doi               10.1021/acs.organomet.5b00537
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C20 H25 N O2 W'
_chemical_formula_sum            'C20 H25 N O2 W'
_chemical_formula_weight         495.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.175(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1177(19)
_cell_length_b                   7.8813(9)
_cell_length_c                   15.4847(19)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.511
_cell_measurement_theta_min      2.716
_cell_volume                     1830.5(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         2.652
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.322
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0933 before and 0.0394 after correction.
The Ratio of minimum to maximum transmission is 0.7071.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       Plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.862
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4227
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.282
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+10.7003P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3932
_reflns_number_total             4227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00537_si_003.cif
_cod_data_source_block           11
_cod_database_code               4087717
_shelxl_version_number           2012-9
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.301
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10A(0.037) H10B(0.037) H10C(0.037) H7A(0.036) H7B(0.036)
 H7C(0.036) H6A(0.034) H6B(0.034) H6C(0.034) H8A(0.037) H8B(0.037) H8C(0.037)
 H9A(0.041) H9B(0.041) H9C(0.041) H12A(0.033) H12B(0.033) H12C(0.033)
 H12D(0.033) H12E(0.033) H12F(0.033) H13(0.02) H14(0.017) H16(0.025) H17(0.028)
 H18(0.031) H19(0.029) H20(0.025) H16A(0.025) H17A(0.028) H18A(0.031)
 H19A(0.029) H20A(0.025) H50A(0.017) H51A(0.02)
 Fixed X: H10A(0.0913) H10B(0.0814) H10C(0.1773) H7A(0.307) H7B(0.2314)
 H7C(0.2263) H6A(0.2898) H6B(0.2507) H6C(0.3267) H8A(0.1127) H8B(0.0376)
 H8C(0.0228) H9A(-0.0284) H9B(-0.0588) H9C(-0.0065) H12A(0.3126) H12B(0.3674)
 H12C(0.2611) H12D(0.2677) H12E(0.3716) H12F(0.3008) H13(0.3442) H14(0.3706)
 H16(0.4624) H17(0.5663) H18(0.5871) H19(0.504) H20(0.4001) H16A(0.4148)
 H17A(0.5191) H18A(0.5844) H19A(0.5454) H20A(0.4412) H50A(0.3564) H51A(0.3547)
 Fixed Y: H10A(0.0163) H10B(-0.1812) H10C(-0.1037) H7A(-0.0897) H7B(-0.2245)
 H7C(-0.0351) H6A(-0.2143) H6B(-0.3493) H6C(-0.2193) H8A(0.1778) H8B(0.0337)
 H8C(0.2077) H9A(0.2218) H9B(0.0426) H9C(0.1752) H12A(0.0897) H12B(0.2533)
 H12C(0.2619) H12D(0.1452) H12E(0.1903) H12F(0.3344) H13(0.3905) H14(0.0444)
 H16(-0.0306) H17(0.0424) H18(0.3272) H19(0.539) H20(0.466) H16A(-0.0097) H17A(-
 0.0654) H18A(0.1591) H19A(0.4393) H20A(0.495) H50A(0.4034) H51A(0.0593)
 Fixed Z: H10A(0.0358) H10B(0.0565) H10C(0.0463) H7A(0.3893) H7B(0.4047)
 H7C(0.4411) H6A(0.1476) H6B(0.2102) H6C(0.2491) H8A(0.4149) H8B(0.4036)
 H8C(0.3505) H9A(0.2099) H9B(0.1676) H9C(0.1143) H12A(0.0535) H12B(0.0296)
 H12C(0.0247) H12D(0.0252) H12E(0.0328) H12F(0.0487) H13(0.1592) H14(0.1993)
 H16(0.3285) H17(0.4476) H18(0.4878) H19(0.4089) H20(0.2898) H16A(0.2826)
 H17A(0.4041) H18A(0.4881) H19A(0.4506) H20A(0.3291) H50A(0.1953) H51A(0.1564)
;
_shelx_res_checksum              26848
_shelx_hkl_checksum              32703
_olex2_submission_special_instructions 'No special instructions were received'