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_4086162
_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         'C20 H36 N2 O2 W'
_chemical_formula_sum            'C20 H36 N2 O2 W'
_chemical_formula_weight         520.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                80.986(3)
_cell_angle_beta                 78.527(3)
_cell_angle_gamma                74.162(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9811(9)
_cell_length_b                   9.0684(10)
_cell_length_c                   15.7146(18)
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.128
_cell_measurement_theta_min      3.192
_cell_volume                     1066.0(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_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  0.0247
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21387
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.152
_diffrn_reflns_theta_min         2.348
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.433
_exptl_absorpt_correction_T_max  0.337
_exptl_absorpt_correction_T_min  0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0694 before and 0.0357 after correction.
The Ratio of minimum to maximum transmission is 0.7229.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       irregular
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.427
_refine_diff_density_min         -3.382
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.429
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         6272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.429
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+6.1106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5962
_reflns_number_total             6272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00426_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               4086162
_shelx_estimated_absorpt_t_max   0.410
_shelx_estimated_absorpt_t_min   0.275
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.034) H6B(0.034) H6C(0.034) H7A(0.03) H7B(0.03) H7C(0.03)
 H8A(0.025) H8B(0.025) H8C(0.025) H9A(0.031) H9B(0.031) H9C(0.031) H10A(0.036)
 H10B(0.036) H10C(0.036) H11A(0.022) H11B(0.022) H12A(0.023) H12B(0.023)
 H13(0.03) H14A(0.069) H14B(0.069) H14C(0.069) H15A(0.058) H15B(0.058)
 H15C(0.058) H16A(0.021) H16B(0.021) H17A(0.021) H17B(0.021) H18A(0.025)
 H18B(0.025) H19A(0.019) H19B(0.019) H20A(0.021) H20B(0.021)
 Fixed X: H6A(0.1177) H6B(0.1054) H6C(0.0947) H7A(0.5163) H7B(0.4454)
 H7C(0.3121) H8A(0.9084) H8B(0.8265) H8C(0.7971) H9A(0.7443) H9B(0.7735)
 H9C(0.8816) H10A(0.2328) H10B(0.378) H10C(0.4157) H11A(0.582) H11B(0.5573)
 H12A(0.2403) H12B(0.2739) H13(0.3538) H14A(0.0466) H14B(0.1082) H14C(0.0661)
 H15A(0.3797) H15B(0.4008) H15C(0.5416) H16A(0.6544) H16B(0.797) H17A(0.877)
 H17B(0.9194) H18A(1.0656) H18B(1.1524) H19A(0.5907) H19B(0.6687) H20A(0.8305)
 H20B(0.8738)
 Fixed Y: H6A(0.8603) H6B(0.9232) H6C(0.7501) H7A(0.8741) H7B(1.0218)
 H7C(0.9253) H8A(0.705) H8B(0.8842) H8C(0.8136) H9A(0.5055) H9B(0.671)
 H9C(0.5746) H10A(0.6533) H10B(0.7044) H10C(0.532) H11A(0.2566) H11B(0.3663)
 H12A(0.4289) H12B(0.3029) H13(0.2326) H14A(0.3059) H14B(0.1288) H14C(0.1724)
 H15A(0.022) H15B(-0.0295) H15C(0.0496) H16A(0.5332) H16B(0.5814) H17A(0.2515)
 H17B(0.4159) H18A(0.3311) H18B(0.2157) H19A(0.2907) H19B(0.1719) H20A(0.0933)
 H20B(0.2584)
 Fixed Z: H6A(0.7122) H6B(0.8035) H6C(0.8016) H7A(0.5597) H7B(0.6129)
 H7C(0.6016) H8A(0.6721) H8B(0.6829) H8C(0.6015) H9A(0.8859) H9B(0.892)
 H9C(0.8128) H10A(0.9232) H10B(0.9609) H10C(0.9369) H11A(0.7812) H11B(0.8555)
 H12A(0.8573) H12B(0.7912) H13(0.965) H14A(0.9651) H14B(1.003) H14C(0.9055)
 H15A(0.8434) H15B(0.9436) H15C(0.8792) H16A(0.5318) H16B(0.5789) H17A(0.7288)
 H17B(0.6958) H18A(0.5606) H18B(0.6372) H19A(0.5728) H19B(0.6506) H20A(0.5163)
 H20B(0.4887)
;
_shelx_res_checksum              35006
_shelx_hkl_checksum              93884
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'