Isomerization Dynamics and Control of the η2/N Equilibrium for Pyridine Complexes
David A. Delafuente; George W. Kosturko; Peter M. Graham; W. Hill Harman; William H. Myers; Yogesh Surendranath; Rachel C. Klet; Kevin D. Welch; Carl O. Trindle; Michal Sabat; W. Dean Harman; Journal of the American Chemical Society 129 (2007) 406–416; doi:10.1021/ja066623f

data_4108973
_publ_section_title
;
 Isomerization Dynamics and Control of the \h2/N Equilibrium for Pyridine
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              406
_journal_page_last               416
_journal_paper_doi               10.1021/ja066623f
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C22 H31 B F3 N8 O6 P S W'
_chemical_formula_weight         818.24
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.734(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0843(7)
_cell_length_b                   14.9833(8)
_cell_length_c                   16.5629(9)
_cell_measurement_reflns_used    9288
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.494
_cell_measurement_theta_min      2.288
_cell_volume                     2946.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40372
_diffrn_reflns_theta_full        32.53
_diffrn_reflns_theta_max         32.53
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    4.117
_exptl_absorpt_correction_T_max  0.801932
_exptl_absorpt_correction_T_min  0.680527
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.258
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         10574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                8403
_reflns_number_total             10574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066623fsi20061101_023601.cif
_cod_data_source_block           C22H31BN8O6F3PSW
_cod_database_code               4108973