Efficient Synthesis of an η2-Pyridine Complex and a Preliminary Investigation of the Bound Heterocycle's Reactivity
Daniel P. Harrison; Kevin D. Welch; Adam C. Nichols-Nielander; Michal Sabat; William H. Myers; W. Dean Harman; Journal of the American Chemical Society 130 (2008) 16844–16845; doi:10.1021/ja807521d

data_4108848
_publ_section_title
;
 Efficient Synthesis of an \h2-Pyridine Complex and a Preliminary
 Investigation of the Bound Heterocycle's Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16844
_journal_page_last               16845
_journal_paper_doi               10.1021/ja807521d
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C20 H27 B F3 N8 O5 P S W'
_chemical_formula_weight         774.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6919(3)
_cell_length_b                   18.7778(7)
_cell_length_c                   19.2958(7)
_cell_measurement_reflns_used    9658
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.203
_cell_measurement_theta_min      2.373
_cell_volume                     2787.03(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37270
_diffrn_reflns_theta_full        32.51
_diffrn_reflns_theta_max         32.51
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.344
_exptl_absorpt_correction_T_max  0.801926
_exptl_absorpt_correction_T_min  0.582882
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS  '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.801
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         10053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                8513
_reflns_number_total             10053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807521d_si_003.cif
_cod_data_source_block           c20h27bf3n8o5psw
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'npt 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_database_code               4108848