Characteristic Spin-Orbit Induced 1H(CH2) Chemical Shifts upon Deprotonation of Group 9 Polyamine Aqua and Alcohol Complexes
Marja Hyvärinen; Juha Vaara; Anna Goldammer; Barbara Kutzky; Kaspar Hegetschweiler; Martin Kaupp; Michal Straka; Journal of the American Chemical Society 131 (2009) 11909–11918; doi:10.1021/ja903637m

data_4104900
_publ_section_title
;
 Characteristic Spin-Orbit Induced 1H(CH2) Chemical Shifts upon
 Deprotonation of Group 9 Polyamine Aqua and Alcohol Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11909
_journal_page_last               11918
_journal_paper_doi               10.1021/ja903637m
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C12 H36 Cl8 N8 O2 Rh2 Zn'
_chemical_formula_weight         879.28
_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                   7.1150(10)
_cell_length_b                   20.084(4)
_cell_length_c                   20.490(4)
_cell_measurement_temperature    200(2)
_cell_volume                     2928.0(9)
_computing_cell_refinement       'STOE IPDS Software, Vers.2.87, 1997'
_computing_data_collection       'STOE IPDS Software, Vers.2.87, 1997'
_computing_data_reduction        'STOE IPDS Software, Vers.2.87, 1997'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'image plate'
_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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18402
_diffrn_reflns_theta_full        23.96
_diffrn_reflns_theta_max         23.96
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.684
_exptl_absorpt_correction_T_max  0.7751
_exptl_absorpt_correction_T_min  0.3471
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                4280
_reflns_number_total             4534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903637m_si_002.cif
_cod_data_source_block           sh2105
_cod_database_code               4104900