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_4064573
_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            'C19 H28 B F3 N7 O4 P S W'
_chemical_formula_weight         733.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.74
_cell_angle_beta                 91.44
_cell_angle_gamma                95.99
_cell_formula_units_Z            2
_cell_length_a                   10.0746(2)
_cell_length_b                   10.1020(2)
_cell_length_c                   12.6597(2)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      36.23
_cell_measurement_theta_min      2.53
_cell_volume                     1279.34(4)
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14881
_diffrn_reflns_theta_full        36.85
_diffrn_reflns_theta_max         36.85
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    4.722
_exptl_absorpt_correction_T_max  0.5187
_exptl_absorpt_correction_T_min  0.2740
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.031
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.554
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.554
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0187
_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          0.0590
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                7531
_reflns_number_total             12304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200183m_si_002.cif
_cod_data_source_block           C19H28BF3N7O4PSW
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        1279.33(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064573