Solid-State 15N CPMAS NMR and Computational Analysis of Ligand Hapticity in Rhodium(η-diene) Poly(pyrazolyl)borate Complexes
Riccardo Pettinari; Claudio Pettinari; Fabio Marchetti; Roberto Gobetto; Carlo Nervi; Michele R. Chierotti; Eric J. Chan; Brian W. Skelton; Allan H. White; Inorganic Chemistry 49 (2010) 11205–11215; doi:10.1021/ic101830e

data_4317212
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   35 Stirling Highway
   Crawley
   Western Australia 6009
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_6488_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08_6488_7107
_publ_section_title
;
 Solid-State 15N CPMAS NMR and Computational Analysis of Ligand Hapticity
 in Rhodium(\h-diene) Poly(pyrazolyl)borate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11205
_journal_page_last               11215
_journal_paper_doi               10.1021/ic101830e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C28 H24  B1 N6 Rh1, C4 H8 O'
_chemical_formula_sum            'C32 H32 B N6 O Rh'
_chemical_formula_weight         630.36
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-03-28T11:29:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.289(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.541(4)
_cell_length_b                   10.734(4)
_cell_length_c                   14.070(6)
_cell_measurement_reflns_used    4815
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.27
_cell_volume                     1360.1(10)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    xtal
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .067
_diffrn_reflns_av_unetI/netI     0.1102
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5861
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_crystal_size_max          .64
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .03
_refine_diff_density_max         1.332
_refine_diff_density_min         -3.156
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.34(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5861
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0897
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+23.9298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2208
_refine_ls_wR_factor_ref         0.2263
_reflns_number_gt                4761
_reflns_number_total             5861
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic101830e_si_001.cif
_cod_data_source_block           cprh8x
_cod_original_sg_symbol_Hall     p_2yb
_cod_database_code               4317212