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_4069715
_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            'C24.5 H32.5 B Cl1.5 N8 O4 P W'
_chemical_formula_weight         781.89
_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                109.535(2)
_cell_angle_beta                 99.029(1)
_cell_angle_gamma                92.124(2)
_cell_formula_units_Z            4
_cell_length_a                   13.096(1)
_cell_length_b                   14.734(1)
_cell_length_c                   16.835(1)
_cell_measurement_reflns_used    6923
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.990
_cell_measurement_theta_min      2.274
_cell_volume                     3009.5(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 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36336
_diffrn_reflns_theta_full        31.12
_diffrn_reflns_theta_max         31.12
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.6670
_exptl_absorpt_correction_T_min  0.5891
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.727
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         18384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                24059
_reflns_number_total             36336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900381c_si_001.cif
_cod_data_source_block           C24H32BN8O4PW.CHCl3
_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_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C24.50 H32.50 B Cl1.50 N8 O4 P W'
_cod_database_code               4069715