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_4069718
_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            'C12 H13 N O4'
_chemical_formula_weight         235.23
_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                 91.1780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2620(10)
_cell_length_b                   6.2710(10)
_cell_length_c                   24.808(2)
_cell_measurement_reflns_used    356
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.568
_cell_measurement_theta_min      3.263
_cell_volume                     1129.5(3)
_computing_cell_refinement       '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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            7515
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.138
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1500
_reflns_number_gt                5574
_reflns_number_total             7515
_reflns_threshold_expression
'>2sigma(I) computing_data_collection Bruker SMART'
_cod_data_source_file            om900381c_si_004.cif
_cod_data_source_block           C12H13NO4
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1129.5(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4069718