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_4086164
_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         'C13.01 H20.02 Cl1 N1 O1 W'
_chemical_formula_sum            'C13.01 H20.02 Cl N O W'
_chemical_formula_weight         425.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5405(3)
_cell_length_b                   10.9050(3)
_cell_length_c                   13.2198(4)
_cell_measurement_reflns_used    9681
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.42
_cell_volume                     1375.38(7)
_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, 2015)'
_diffrn_ambient_temperature      100(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and X8 diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17334
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.074
_diffrn_reflns_theta_min         2.421
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.578
_exptl_absorpt_correction_T_max  0.276
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0616 before and 0.0396 after correction.
The Ratio of minimum to maximum transmission is 0.8575.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_description       prism
_exptl_crystal_F_000             817
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.427(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4035
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+3.3649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0415
_reflns_Friedel_coverage         0.757
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                3910
_reflns_number_total             4035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00426_si_002.cif
_cod_data_source_block           10
_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               4086164
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.048) H6B(0.048) H6C(0.048) H7A(0.049) H7B(0.049) H7C(0.049)
 H8A(0.056) H8B(0.056) H8C(0.056) H9A(0.049) H9B(0.049) H9C(0.049) H10A(0.052)
 H10B(0.052) H10C(0.052) H11A(0.033) H11B(0.033) H12(0.029) H13A(0.034)
 H13B(0.034) H11C(0.033) H11D(0.033) H12A(0.029) H13C(0.034) H13D(0.034)
 H11E(0.033) H11F(0.033) H12B(0.029) H13E(0.034) H13F(0.034)
 Fixed X: H6A(0.2585) H6B(0.395) H6C(0.3148) H7A(0.4524) H7B(0.6135)
 H7C(0.5543) H8A(0.6668) H8B(0.7825) H8C(0.7082) H9A(0.6443) H9B(0.6641)
 H9C(0.5221) H10A(0.3607) H10B(0.4622) H10C(0.311) H11A(0.141) H11B(0.151)
 H12(0.0514) H13A(0.1048) H13B(0.1038) H11C(0.1015) H11D(0.11) H12A(0.0617)
 H13C(0.1638) H13D(0.1439) H11E(0.0675) H11F(0.0697) H12B(0.0815) H13E(0.1616)
 H13F(0.199)
 Fixed Y: H6A(-0.2779) H6B(-0.3372) H6C(-0.2364) H7A(-0.0939) H7B(-0.1171)
 H7C(0.0169) H8A(0.1328) H8B(0.0441) H8C(0.1368) H9A(0.0601) H9B(-0.0776) H9C(-
 0.0107) H10A(-0.1919) H10B(-0.2945) H10C(-0.2829) H11A(-0.1443) H11B(-0.0573)
 H12(0.0972) H13A(0.1099) H13B(-0.039) H11C(-0.0108) H11D(0.1366) H12A(0.109)
 H13C(-0.0515) H13D(-0.1363) H11E(0.0652) H11F(0.1575) H12B(-0.0972)
 H13E(0.0458) H13F(-0.0978)
 Fixed Z: H6A(0.4416) H6B(0.3973) H6C(0.3356) H7A(0.2609) H7B(0.2742)
 H7C(0.2781) H8A(0.406) H8B(0.4477) H8C(0.5207) H9A(0.6735) H9B(0.7044)
 H9C(0.7272) H10A(0.697) H10B(0.6579) H10C(0.6126) H11A(0.5456) H11B(0.6444)
 H12(0.5466) H13A(0.376) H13B(0.376) H11C(0.6302) H11D(0.6152) H12A(0.4438)
 H13C(0.359) H13D(0.4579) H11E(0.5986) H11F(0.5022) H12B(0.4919) H13E(0.3295)
 H13F(0.3453)
;
_shelx_res_checksum              18611
_shelx_hkl_checksum              9300
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'