Functionalization of Methane Initiated by Cp*W(NO)(CH2CMe3)(η3-CH2CHCMe2)
Baillie, Rhett A.; Patrick, Brian O.; Legzdins, Peter; Rosenfeld, Devon C.; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00738

data_4086842
_publ_section_title
;
 Functionalization of Methane Initiated by
 Cp*W(NO)(CH2CMe3)(\h3-CH2CHCMe2)
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00738
_journal_year                    2016
_chemical_formula_moiety         'C17 H27 N O2 W'
_chemical_formula_sum            'C17 H27 N O2 W'
_chemical_formula_weight         461.24
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.412(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0573(19)
_cell_length_b                   14.9969(17)
_cell_length_c                   15.4854(18)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.464
_cell_measurement_theta_min      2.747
_cell_volume                     3395.6(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40967
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.464
_diffrn_reflns_theta_min         1.393
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.808
_exptl_absorpt_correction_T_max  0.473
_exptl_absorpt_correction_T_min  0.368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0771 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.7788.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.671
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6990
_refine_ls_number_restraints     681
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+24.5516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5020
_reflns_number_total             6990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00738_si_008.cif
_cod_data_source_block           pl423b/5
_cod_database_code               4086842
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 W2B-W2
 0.2 with sigma of 0.02
 O4-C33
 1.2 with sigma of 0.01
 C34-C33 \\sim C17-C16
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(W1) = Uanis(W1B)
Uanis(W2) = Uanis(W2B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(W1B)=1-FVAR(1)
 Sof(W1)=FVAR(1)
 Sof(W2B)=1-FVAR(2)
 Sof(W2)=FVAR(2)
6.a Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C10(H10A,H10B,H10C), C27(H27A,H27B,
 H27C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C32(H32A,H32B,H32C),
 C34(H34A,H34B,H34C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C17(H17A,H17B,
 H17C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C), C24(H24A,
 H24B,H24C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'