Hyperdistorted Tungsten Allyl Complexes and Their Stereoselective Deprotonation to Form Dihapto-Coordinated Dienes
Harrison, Daniel P.; Nichols-Nielander, Adam C.; Zottig, Victor E.; Strausberg, Laura; Salomon, Rebecca J.; Trindle, Carl O.; Sabat, Michal; Gunnoe, T. Brent; Iovan, Diana A.; Myers, William H.; Harman, W. Dean; Organometallics 30 (2011) 2587–; doi:10.1021/om200183m

data_4064576
_publ_section_title
;
 Hyperdistorted Tungsten Allyl Complexes and Their Stereoselective
 Deprotonation to Form Dihapto-Coordinated Dienes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2587
_journal_paper_doi               10.1021/om200183m
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C24 H32 B Cl2 F9 N8 O10 P S3 W'
_chemical_formula_weight         1156.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.16(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.966(2)
_cell_length_b                   11.615(1)
_cell_length_c                   21.420(3)
_cell_measurement_reflns_used    1608
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      16.60
_cell_measurement_theta_min      2.29
_cell_volume                     4209.9(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11436
_diffrn_reflns_theta_full        16.68
_diffrn_reflns_theta_max         16.68
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    3.156
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.4976
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00027(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.763
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         2332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                1748
_reflns_number_total             2332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200183m_si_002.cif
_cod_data_source_block           C24H32BCl2F9N8O10PS3W
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4209.9
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C24 H32 B1 Cl2 F9 N8 O10 P S3 W'
_cod_database_code               4064576