Thermal Chemistry of Cp*W(NO)(H)(η3-allyl) Complexes
Baillie, Rhett A.; Wakeham, Russell J.; Lefèvre, Guillaume P.; Béthegnies, Aurélien; Patrick, Brian O.; Legzdins, Peter; Rosenfeld, Devon C.; Organometallics 34 (2015) 3428–; doi:10.1021/acs.organomet.5b00426

data_4086163
_publ_section_title
;
 Thermal Chemistry of Cp*W(NO)(H)(\h3-allyl) Complexes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3428
_journal_paper_doi               10.1021/acs.organomet.5b00426
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C19 H34 N2 O2 W'
_chemical_formula_sum            'C19 H34 N2 O2 W'
_chemical_formula_weight         506.33
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 113.452(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   30.058(3)
_cell_length_b                   8.0516(9)
_cell_length_c                   35.124(3)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.64
_cell_volume                     7798.3(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'OLEX2 (Dolomanov, 2009)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            49037
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_min         1.264
_exptl_absorpt_coefficient_mu    5.938
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.888
_refine_diff_density_min         -2.297
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+115.3546P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8279
_reflns_number_total             9295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00426_si_002.cif
_cod_data_source_block           9
_cod_original_cell_volume        7798.5(14)
_cod_database_code               4086163
_shelxl_version_number           2012-9
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.512
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.03) H6B(0.03) H6C(0.03) H7A(0.036) H7B(0.036) H7C(0.036)
 H8A(0.034) H8B(0.034) H8C(0.034) H9A(0.028) H9B(0.028) H9C(0.028) H10A(0.025)
 H10B(0.025) H10C(0.025) H12A(0.021) H12B(0.021) H13A(0.024) H13B(0.024)
 H14A(0.025) H14B(0.025) H15A(0.022) H15B(0.022) H17A(0.023) H17B(0.023)
 H18A(0.03) H18B(0.03) H19A(0.046) H19B(0.046) H19C(0.046) H25A(0.023)
 H25B(0.023) H25C(0.023) H26A(0.024) H26B(0.024) H26C(0.024) H27A(0.024)
 H27B(0.024) H27C(0.024) H28A(0.028) H28B(0.028) H28C(0.028) H29A(0.026)
 H29B(0.026) H29C(0.026) H31A(0.017) H31B(0.017) H32A(0.02) H32B(0.02)
 H33A(0.022) H33B(0.022) H34A(0.016) H34B(0.016) H36A(0.015) H36B(0.015)
 H37A(0.018) H37B(0.018) H38A(0.031) H38B(0.031) H38C(0.031)
 Fixed X: H6A(0.4449) H6B(0.4471) H6C(0.4608) H7A(0.3252) H7B(0.341)
 H7C(0.3814) H8A(0.2317) H8B(0.2418) H8C(0.252) H9A(0.2954) H9B(0.2849)
 H9C(0.2517) H10A(0.4338) H10B(0.3928) H10C(0.3904) H12A(0.357) H12B(0.3921)
 H13A(0.3464) H13B(0.2971) H14A(0.2727) H14B(0.3053) H15A(0.3658) H15B(0.3152)
 H17A(0.4607) H17B(0.4875) H18A(0.4325) H18B(0.4075) H19A(0.4803) H19B(0.4604)
 H19C(0.5044) H25A(0.4569) H25B(0.4768) H25C(0.5008) H26A(0.3243) H26B(0.3458)
 H26C(0.373) H27A(0.3066) H27B(0.3053) H27C(0.2908) H28A(0.422) H28B(0.4082)
 H28C(0.3664) H29A(0.5183) H29B(0.5104) H29C(0.4965) H31A(0.429) H31B(0.3767)
 H32A(0.4314) H32B(0.4674) H33A(0.4451) H33B(0.3936) H34A(0.353) H34B(0.3916)
 H36A(0.2634) H36B(0.3053) H37A(0.309) H37B(0.3431) H38A(0.2415) H38B(0.2838)
 H38C(0.2735)
 Fixed Y: H6A(0.9457) H6B(0.8674) H6C(0.7561) H7A(1.1138) H7B(1.1378)
 H7C(1.1154) H8A(0.7837) H8B(0.8805) H8C(0.9698) H9A(0.3929) H9B(0.4756)
 H9C(0.5217) H10A(0.5062) H10B(0.4648) H10C(0.3828) H12A(1.0469) H12B(0.9617)
 H13A(1.1716) H13B(1.0847) H14A(0.8312) H14B(0.7425) H15A(0.6852) H15B(0.6081)
 H17A(0.5231) H17B(0.556) H18A(0.3714) H18B(0.3352) H19A(0.2163) H19B(0.1207)
 H19C(0.2492) H25A(0.4418) H25B(0.4727) H25C(0.5683) H26A(0.5219) H26B(0.4462)
 H26C(0.4136) H27A(0.9511) H27B(0.7696) H27C(0.7945) H28A(1.1669) H28B(1.1024)
 H28C(1.1378) H29A(0.8501) H29B(0.883) H29C(1.0236) H31A(0.9331) H31B(0.8573)
 H32A(0.7962) H32B(0.7073) H33A(0.4525) H33B(0.3704) H34A(0.5838) H34B(0.4991)
 H36A(1.0019) H36B(1.0616) H37A(1.1313) H37B(1.2114) H38A(1.2763) H38B(1.407)
 H38C(1.3486)
 Fixed Z: H6A(0.2201) H6B(0.179) H6C(0.2199) H7A(0.1999) H7B(0.1618)
 H7C(0.2078) H8A(0.1525) H8B(0.1169) H8C(0.1603) H9A(0.1555) H9B(0.1113)
 H9C(0.1358) H10A(0.1874) H10B(0.1426) H10C(0.1833) H12A(0.2743) H12B(0.317)
 H13A(0.3307) H13B(0.3004) H14A(0.3184) H14B(0.3614) H15A(0.3365) H15B(0.3053)
 H17A(0.2577) H17B(0.3064) H18A(0.3181) H18B(0.2694) H19A(0.2723) H19B(0.3023)
 H19C(0.3213) H25A(0.0678) H25B(0.1168) H25C(0.0898) H26A(0.0266) H26B(0.0726)
 H26C(0.0423) H27A(0.0675) H27B(0.0857) H27C(0.037) H28A(0.0945) H28B(0.1315)
 H28C(0.0867) H29A(0.1033) H29B(0.1451) H29C(0.1101) H31A(-0.0548) H31B(-
 0.0825) H32A(-0.1135) H32B(-0.0718) H33A(-0.0511) H33B(-0.0784) H34A(-0.0593)
 H34B(-0.0182) H36A(-0.0359) H36B(0.0066) H37A(-0.0718) H37B(-0.0282) H38A(-
 0.0707) H38B(-0.0649) H38C(-0.0256)
;
_shelx_res_checksum              34863
_shelx_hkl_checksum              45028