Spontaneous Transfer of Parahydrogen Derived Spin Order to Pyridine at Low Magnetic Field
Kevin D. Atkinson; Michael J. Cowley; Paul I. P. Elliott; Simon B. Duckett; Gary G. R. Green; Joaquín López-Serrano; Adrian C. Whitwood; Journal of the American Chemical Society 131 (2009) 13362–13368; doi:10.1021/ja903601p

data_4105022
_publ_contact_author_address
;Department of Chemistry,
University of York,
Heslington,
York, YO10 5DD.
UK.
;
_publ_contact_author_email       sbd3@york.ac.uk
_publ_contact_author_name        'Prof Simon B Duckett'
_publ_section_title
;
 Spontaneous Transfer of Parahydrogen Derived Spin Order to Pyridine at
 Low Magnetic Field
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13362
_journal_page_last               13368
_journal_paper_doi               10.1021/ja903601p
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C33 H50 Ir N3 P, B F4'
_chemical_formula_sum            'C33 H50 B F4 Ir N3 P'
_chemical_formula_weight         798.74
_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                95.5650(10)
_cell_angle_beta                 96.4400(10)
_cell_angle_gamma                110.9510(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9232(5)
_cell_length_b                   10.3821(5)
_cell_length_c                   18.0076(8)
_cell_measurement_reflns_used    5284
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.23
_cell_volume                     1702.73(14)
_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, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17642
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    4.016
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10; (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.594
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+1.3952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0488
_reflns_number_gt                7812
_reflns_number_total             8390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903601p_si_001.cif
_cod_data_source_block           sbd0807m
_cod_database_code               4105022