Stereoelectronic Effects in Dihapto-Coordinated Complexes of TpW(NO)(PMe3) and Their Manifestation in Diels-Alder Cycloaddition of Arenes
Salomon, Rebecca J.; Lis, Jr., Edward C.; Kasbekar, Monica U.; Bassett, Kimberley C.; Myers, William H.; Trindle, Carl O.; Sabat, Michal; Harman, W. Dean; Organometallics 28 (2009) 4724–4734; doi:10.1021/om900381c

data_4069717
_publ_section_title
;
 Stereoelectronic Effects in Dihapto-Coordinated Complexes of
 TpW(NO)(PMe3) and Their Manifestation in Diels-Alder Cycloaddition
 of Arenes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4724
_journal_page_last               4734
_journal_paper_doi               10.1021/om900381c
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C23 H32 B N8 O3 P W'
_chemical_formula_weight         694.20
_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                 99.534(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.136(1)
_cell_length_b                   13.210(1)
_cell_length_c                   19.493(2)
_cell_measurement_reflns_used    5823
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.551
_cell_measurement_theta_min      2.524
_cell_volume                     2574.0(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.1012
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14525
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    4.593
_exptl_absorpt_correction_T_max  0.8324
_exptl_absorpt_correction_T_min  0.6199
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.532
_refine_diff_density_min         -1.801
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         14525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                8658
_reflns_number_total             14525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900381c_si_003.cif
_cod_data_source_block           C23H32BN8O3PW
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2574.0(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4069717