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_4317216
_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         'C17 H22 B N6 Rh'
_chemical_formula_sum            'C17 H22 B N6 Rh'
_chemical_formula_weight         424.13
_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_date             2008-03-18T09:28:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.512(2)
_cell_angle_beta                 92.130(2)
_cell_angle_gamma                93.378(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2506(7)
_cell_length_b                   7.5215(8)
_cell_length_c                   15.866(2)
_cell_measurement_reflns_used    5370
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.5
_cell_measurement_theta_min      2.64
_cell_volume                     838.69(16)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    xtal
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.969
_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  0.020
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8596
_diffrn_reflns_theta_full        35
_diffrn_reflns_theta_max         37.55
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_exptl_crystal_size_max          .24
_exptl_crystal_size_mid          .13
_exptl_crystal_size_min          .12
_refine_diff_density_max         3.299
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         8596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.6888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.094
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                7696
_reflns_number_total             8596
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic101830e_si_005.cif
_cod_data_source_block           cprh54
_cod_original_sg_symbol_Hall     -p_1
_cod_database_code               4317216