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_4086161
_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         'C15 H24 N O W'
_chemical_formula_sum            'C15 H25 N O W'
_chemical_formula_weight         419.21
_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             2014-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.748(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.181(2)
_cell_length_b                   8.1358(18)
_cell_length_c                   18.596(4)
_cell_measurement_reflns_used    8083
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      3.23
_cell_volume                     1518.1(6)
_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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(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 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX2 area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19588
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.069
_diffrn_reflns_theta_min         2.030
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.599
_exptl_absorpt_correction_T_max  0.402
_exptl_absorpt_correction_T_min  0.307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0990 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.7651.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       irregular
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.232
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0199P)^2^+2.9177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3853
_reflns_number_total             4439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00426_si_002.cif
_cod_data_source_block           4a
_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               4086161
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.462
_shelx_estimated_absorpt_t_min   0.274
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.031) H6B(0.031) H6C(0.031) H7A(0.03) H7B(0.03) H7C(0.03)
 H8A(0.034) H8B(0.034) H8C(0.034) H9A(0.034) H9B(0.034) H9C(0.034) H10A(0.034)
 H10B(0.034) H10C(0.034) H14A(0.028) H14B(0.028) H15A(0.043) H15B(0.043)
 H15C(0.043)
 Fixed X: H6A(0.7711) H6B(0.6291) H6C(0.6371) H7A(0.9651) H7B(0.8587)
 H7C(0.9136) H8A(0.7996) H8B(0.7708) H8C(0.9046) H9A(0.4809) H9B(0.4787)
 H9C(0.5951) H10A(0.4747) H10B(0.3875) H10C(0.4317) H14A(0.8041) H14B(0.8639)
 H15A(0.5991) H15B(0.6355) H15C(0.6587)
 Fixed Y: H6A(0.3141) H6B(0.2297) H6C(0.4166) H7A(0.2546) H7B(0.1112)
 H7C(0.2156) H8A(0.4963) H8B(0.3029) H8C(0.3746) H9A(0.673) H9B(0.5061)
 H9C(0.6375) H10A(0.5717) H10B(0.4704) H10C(0.6551) H14A(0.9774) H14B(0.9106)
 H15A(0.8447) H15B(0.9636) H15C(0.7697)
 Fixed Z: H6A(0.4775) H6B(0.451) H6C(0.4782) H7A(0.3292) H7B(0.3323)
 H7C(0.404) H8A(0.1674) H8B(0.1668) H8C(0.214) H9A(0.2142) H9B(0.1685)
 H9C(0.1668) H10A(0.4082) H10B(0.3433) H10C(0.3298) H14A(0.4618) H14B(0.5414)
 H15A(0.4667) H15B(0.5358) H15C(0.545)
;
_shelx_res_checksum              78655
_shelx_hkl_checksum              91701
_olex2_submission_special_instructions 'No special instructions were received'