Observation of Intramolecular Paramagnetic T1 Spin Decoupling in the 13C NMR Spectra of Triazacyclohexane Complexes of Ni(II)
Randolf Dag Köhn; Matthias Haufe; Gabriele Kociok-Köhn; Journal of the American Chemical Society 128 (2006) 10682–10683; doi:10.1021/ja063357x

data_4110820
_publ_contact_author_address
;Department of Chemistry
University of Bath
Bath, BA2 7AY
United Kingdom
;
_publ_contact_author_email       r.d.kohn@bath.ac.uk
_publ_contact_author_fax         '# 44 1225 82 6231'
_publ_contact_author_name        'Randolf Dag K\"ohn'
_publ_contact_author_phone       '# 44 1225 38 3305'
_publ_section_title
;
 Observation of Intramolecular Paramagnetic T1 Spin Decoupling in the 13C
 NMR Spectra of Triazacyclohexane Complexes of Ni(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10682
_journal_page_last               10683
_journal_paper_doi               10.1021/ja063357x
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C30 H36 N6 Ni 1+, B2 F8 1-'
_chemical_formula_sum            'C30 H36 B2 F8 N6 Ni'
_chemical_formula_weight         712.98
_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                71.5000(10)
_cell_angle_beta                 71.1650(10)
_cell_angle_gamma                71.6250(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9500(2)
_cell_length_b                   10.9920(2)
_cell_length_c                   16.3930(4)
_cell_measurement_reflns_used    37097
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.575
_cell_measurement_theta_min      2.910
_cell_volume                     1720.45(6)
_computing_cell_refinement
'Collect, Nonius program suite version 1.9 (1997)'
_computing_data_collection
'Collect, Nonius program suite version 1.9 (1997)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material  'SHELX97-2, G. M. Sheldrick'
_computing_structure_refinement
;
 SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick,
 Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4, 
 D-3400 G\"ottingen, Germany, 1998.
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '228 1.9 degree images with \w 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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33304
_diffrn_reflns_theta_full        29.60
_diffrn_reflns_theta_max         29.60
_diffrn_reflns_theta_min         3.83
_diffrn_standards_decay_%        -0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'intense blue'
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0503P)^2^+0.4527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                7066
_reflns_number_total             9592
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063357xsi20060515_043723.cif
_cod_data_source_block           h06rdk1
_cod_database_code               4110820