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_4317215
_publ_contact_author_address
;
 Chemistry, 
School of Biomedical, Biomolecular and Chemical Science, 
M313, University of Western Australia, 
Perth, WA 6009,
 Australia
;
_publ_contact_author_email       brian.skelton@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         'C43 H36 B N6 Rh, C4 H10 O'
_chemical_formula_sum            'C47 H46 B N6 O Rh'
_chemical_formula_weight         824.62
_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             2010-07-04T16:05:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.865(2)
_cell_angle_beta                 85.610(2)
_cell_angle_gamma                65.513(2)
_cell_formula_units_Z            4
_cell_length_a                   13.6255(3)
_cell_length_b                   14.9316(3)
_cell_length_c                   21.0256(4)
_cell_measurement_reflns_used    51016
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.0427
_cell_measurement_theta_min      2.8772
_cell_volume                     3881.42(15)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0401643117
_diffrn_orient_matrix_UB_12      0.0482691469
_diffrn_orient_matrix_UB_13      -0.0043529761
_diffrn_orient_matrix_UB_21      -0.0098634888
_diffrn_orient_matrix_UB_22      -0.013816843
_diffrn_orient_matrix_UB_23      -0.029948879
_diffrn_orient_matrix_UB_31      -0.0396532263
_diffrn_orient_matrix_UB_32      -0.0142618174
_diffrn_orient_matrix_UB_33      0.0151125089
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            132902
_diffrn_reflns_theta_full        36.5
_diffrn_reflns_theta_max         37.1
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
         CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.243
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         38578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                27575
_reflns_number_total             38578
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101830e_si_004.cif
_cod_data_source_block           cprh12a
_cod_original_cell_volume        3881.42(14)
_cod_original_sg_symbol_Hall     -p_1
_cod_database_code               4317215