#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317216.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4317216
loop_
_publ_author_name
'Riccardo Pettinari'
'Claudio Pettinari'
'Fabio Marchetti'
'Roberto Gobetto'
'Carlo Nervi'
'Michele R. Chierotti'
'Eric J. Chan'
'Brian W. Skelton'
'Allan H. White'
_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(η-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
_chemical_name_systematic
;
 ?
;
_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       'ω 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/[σ²(Fo²)+(0.0477P)²+0.6888P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh Rh 0.339169(18) 0.434275(17) 0.220232(8) 0.01503(4) Uani 1 1 d . B .
N12 N 0.2552(2) 0.6760(2) 0.32034(10) 0.0174(2) Uani 1 1 d . . .
N11 N 0.3867(2) 0.8018(2) 0.36518(10) 0.0157(2) Uani 1 1 d . . .
C15 C 0.3075(2) 0.9464(2) 0.41267(11) 0.0179(3) Uani 1 1 d . . .
H15 H 0.3711 1.052 0.4494 0.021 Uiso 1 1 calc R . .
C14 C 0.1182(3) 0.9157(3) 0.39913(12) 0.0213(3) Uani 1 1 d . . .
H14 H 0.0258 0.9934 0.4239 0.026 Uiso 1 1 calc R . .
C13 C 0.0929(2) 0.7445(3) 0.34066(12) 0.0206(3) Uani 1 1 d . . .
H13 H -0.0241 0.685 0.3184 0.025 Uiso 1 1 calc R . .
N22 N 0.5375(2) 0.6230(2) 0.19247(9) 0.0166(2) Uani 1 1 d . . .
N21 N 0.62979(19) 0.7519(2) 0.25694(9) 0.0143(2) Uani 1 1 d . . .
C25 C 0.7473(3) 0.8572(3) 0.22251(12) 0.0214(3) Uani 1 1 d . . .
H25 H 0.8269 0.9572 0.2542 0.026 Uiso 1 1 calc R . .
C24 C 0.7328(4) 0.7956(4) 0.13372(14) 0.0412(7) Uani 1 1 d . . .
H24 H 0.7988 0.8427 0.0921 0.049 Uiso 1 1 calc R . .
C23 C 0.6005(3) 0.6495(4) 0.11838(13) 0.0323(5) Uani 1 1 d . . .
H23 H 0.5602 0.5778 0.0624 0.039 Uiso 1 1 calc R . .
N32 N 0.5474(2) 0.4258(2) 0.32881(10) 0.0185(2) Uani 1 1 d . . .
N31 N 0.6297(2) 0.5866(2) 0.37694(10) 0.0164(2) Uani 1 1 d . . .
C35 C 0.7386(3) 0.5550(3) 0.44205(12) 0.0209(3) Uani 1 1 d . . .
H35 H 0.8101 0.6456 0.4844 0.025 Uiso 1 1 calc R . .
C34 C 0.7287(3) 0.3694(3) 0.43666(14) 0.0253(4) Uani 1 1 d . . .
H34 H 0.7898 0.3062 0.4736 0.03 Uiso 1 1 calc R . .
C33 C 0.6084(3) 0.2950(3) 0.36458(14) 0.0231(3) Uani 1 1 d . . .
H33 H 0.5745 0.1679 0.3437 0.028 Uiso 1 1 calc R . .
B1 B 0.5911(2) 0.7669(3) 0.35327(12) 0.0150(3) Uani 1 1 d . . .
H1 H 0.6711 0.87 0.391 0.018 Uiso 1 1 calc R . .
C1 C 0.0760(3) 0.3056(3) 0.23999(14) 0.0241(3) Uani 1 1 d . B .
H1A H 0.0698 0.4035 0.2898 0.029 Uiso 1 1 calc R . .
C2 C 0.2113(3) 0.1845(3) 0.24186(15) 0.0271(4) Uani 1 1 d . B .
H2 H 0.2908 0.2061 0.2927 0.033 Uiso 1 1 calc R . .
C3 C 0.2427(3) 0.0208(3) 0.1697(2) 0.0378(6) Uani 1 1 d . . .
H3A H 0.3541 -0.037 0.1853 0.045 Uiso 0.5 1 calc PR A 1
H3B H 0.1358 -0.0702 0.1636 0.045 Uiso 0.5 1 calc PR A 1
H3'A H 0.1207 -0.0359 0.1437 0.045 Uiso 0.5 1 d PR A 2
H3'B H 0.3034 -0.0703 0.1952 0.045 Uiso 0.5 1 d PR A 2
C4 C 0.2659(6) 0.0658(5) 0.0904(3) 0.0219(6) Uani 0.5 1 d P B 1
H4A H 0.1434 0.0548 0.0592 0.026 Uiso 0.5 1 calc PR B 1
H4B H 0.3436 -0.0241 0.0551 0.026 Uiso 0.5 1 calc PR B 1
C5 C 0.3577(4) 0.2649(3) 0.09794(13) 0.0285(4) Uani 1 1 d . . .
H5 H 0.4872 0.2959 0.1028 0.034 Uiso 0.5 1 calc PR B 1
H5' H 0.4783 0.3246 0.1039 0.034 Uiso 0.5 1 d PR B 2
C6 C 0.2199(3) 0.3916(3) 0.09646(12) 0.0233(3) Uani 1 1 d . B .
H6 H 0.2722 0.5115 0.0987 0.028 Uiso 0.5 1 calc PR C 1
H6' H 0.2445 0.5195 0.1024 0.028 Uiso 0.5 1 d PR C 2
C7 C 0.0042(5) 0.3818(7) 0.0920(3) 0.0212(6) Uani 0.5 1 d P B 1
H7A H -0.0399 0.5063 0.0993 0.025 Uiso 0.5 1 calc PR B 1
H7B H -0.0451 0.3062 0.035 0.025 Uiso 0.5 1 calc PR B 1
C8 C -0.0621(3) 0.2952(4) 0.16576(18) 0.0316(5) Uani 1 1 d . . .
H8A H -0.173 0.3561 0.1892 0.038 Uiso 0.5 1 calc PR B 1
H8B H -0.1008 0.1646 0.1405 0.038 Uiso 0.5 1 calc PR B 1
H8'A H -0.1454 0.1829 0.1585 0.038 Uiso 0.5 1 d PR B 2
H8'B H -0.1386 0.402 0.1796 0.038 Uiso 0.5 1 d PR B 2
C4' C 0.3666(7) 0.0622(5) 0.0927(3) 0.0233(7) Uani 0.5 1 d P B 2
H4'A H 0.4959 0.0319 0.1012 0.028 Uiso 0.5 1 calc PR B 2
H4'B H 0.3157 -0.0109 0.0355 0.028 Uiso 0.5 1 calc PR B 2
C7' C 0.0267(5) 0.2927(7) 0.0839(3) 0.0228(7) Uani 0.5 1 d P B 2
H7'A H -0.0525 0.3512 0.0475 0.027 Uiso 0.5 1 calc PR B 2
H7'B H 0.0361 0.1638 0.0522 0.027 Uiso 0.5 1 calc PR B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Rh C5 40.30(9) . . ?
C6 Rh N22 90.35(7) . . ?
C5 Rh N22 90.60(8) . . ?
C6 Rh C2 93.55(8) . . ?
C5 Rh C2 80.57(9) . . ?
N22 Rh C2 161.04(8) . . ?
C6 Rh C1 80.81(8) . . ?
C5 Rh C1 93.23(9) . . ?
N22 Rh C1 161.14(8) . . ?
C2 Rh C1 37.42(8) . . ?
C6 Rh N12 117.44(7) . . ?
C5 Rh N12 157.31(7) . . ?
N22 Rh N12 84.28(6) . . ?
C2 Rh N12 110.09(8) . . ?
C1 Rh N12 85.09(7) . . ?
C6 Rh N32 159.70(8) . . ?
C5 Rh N32 120.23(8) . . ?
N22 Rh N32 83.25(6) . . ?
C2 Rh N32 86.75(7) . . ?
C1 Rh N32 110.42(7) . . ?
N12 Rh N32 81.18(6) . . ?
C13 N12 N11 106.26(15) . . ?
C13 N12 Rh 133.38(12) . . ?
N11 N12 Rh 119.67(10) . . ?
C15 N11 N12 110.23(14) . . ?
C15 N11 B1 130.47(15) . . ?
N12 N11 B1 119.25(14) . . ?
N11 C15 C14 108.41(16) . . ?
N11 C15 H15 125.8 . . ?
C14 C15 H15 125.8 . . ?
C15 C14 C13 104.38(15) . . ?
C15 C14 H14 127.8 . . ?
C13 C14 H14 127.8 . . ?
N12 C13 C14 110.73(16) . . ?
N12 C13 H13 124.6 . . ?
C14 C13 H13 124.6 . . ?
C23 N22 N21 106.31(15) . . ?
C23 N22 Rh 132.59(13) . . ?
N21 N22 Rh 121.10(11) . . ?
C25 N21 N22 109.68(14) . . ?
C25 N21 B1 128.77(15) . . ?
N22 N21 B1 121.53(13) . . ?
N21 C25 C24 108.47(17) . . ?
N21 C25 H25 125.8 . . ?
C24 C25 H25 125.8 . . ?
C25 C24 C23 104.61(18) . . ?
C25 C24 H24 127.7 . . ?
C23 C24 H24 127.7 . . ?
N22 C23 C24 110.93(18) . . ?
N22 C23 H23 124.5 . . ?
C24 C23 H23 124.5 . . ?
C33 N32 N31 105.96(15) . . ?
C33 N32 Rh 135.19(14) . . ?
N31 N32 Rh 118.70(11) . . ?
C35 N31 N32 110.08(15) . . ?
C35 N31 B1 129.94(16) . . ?
N32 N31 B1 119.98(13) . . ?
N31 C35 C34 108.42(17) . . ?
N31 C35 H35 125.8 . . ?
C34 C35 H35 125.8 . . ?
C35 C34 C33 104.40(16) . . ?
C35 C34 H34 127.8 . . ?
C33 C34 H34 127.8 . . ?
N32 C33 C34 111.13(18) . . ?
N32 C33 H33 124.4 . . ?
C34 C33 H33 124.4 . . ?
N31 B1 N11 109.15(14) . . ?
N31 B1 N21 109.35(14) . . ?
N11 B1 N21 108.12(13) . . ?
N31 B1 H1 110.1 . . ?
N11 B1 H1 110.1 . . ?
N21 B1 H1 110.1 . . ?
C2 C1 C8 125.4(2) . . ?
C2 C1 Rh 71.12(11) . . ?
C8 C1 Rh 112.12(14) . . ?
C2 C1 H1A 117.3 . . ?
C8 C1 H1A 117.3 . . ?
Rh C1 H1A 86.7 . . ?
C1 C2 C3 125.2(2) . . ?
C1 C2 Rh 71.46(11) . . ?
C3 C2 Rh 112.09(15) . . ?
C1 C2 H2 117.4 . . ?
C3 C2 H2 117.4 . . ?
Rh C2 H2 86.4 . . ?
C4 C3 C2 112.9(2) . . ?
C2 C3 C4' 115.8(2) . . ?
C4 C3 H3A 109 . . ?
C2 C3 H3A 109 . . ?
C4 C3 H3B 109 . . ?
C2 C3 H3B 109 . . ?
H3A C3 H3B 107.8 . . ?
C2 C3 H3'A 108.3 . . ?
C4' C3 H3'A 108.3 . . ?
C2 C3 H3'B 108.3 . . ?
C4' C3 H3'B 108.3 . . ?
H3'A C3 H3'B 107.4 . . ?
C3 C4 C5 114.3(3) . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C6 C5 C4' 138.0(3) . . ?
C6 C5 C4 110.7(3) . . ?
C6 C5 Rh 69.51(11) . . ?
C4' C5 Rh 116.9(2) . . ?
C4 C5 Rh 112.46(19) . . ?
C6 C5 H5 124.6 . . ?
C4 C5 H5 124.6 . . ?
Rh C5 H5 88.4 . . ?
C6 C5 H5' 111 . . ?
C4' C5 H5' 111 . . ?
Rh C5 H5' 81.7 . . ?
C5 C6 C7' 110.5(3) . . ?
C5 C6 C7 135.7(3) . . ?
C5 C6 Rh 70.19(11) . . ?
C7' C6 Rh 114.56(19) . . ?
C7 C6 Rh 114.35(18) . . ?
C5 C6 H6 112.1 . . ?
C7 C6 H6 112.1 . . ?
Rh C6 H6 84.4 . . ?
C5 C6 H6' 124.8 . . ?
C7' C6 H6' 124.8 . . ?
Rh C6 H6' 86.1 . . ?
C8 C7 C6 107.7(3) . . ?
C8 C7 H7A 110.2 . . ?
C6 C7 H7A 110.2 . . ?
C8 C7 H7B 110.2 . . ?
C6 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
C7' C8 C1 112.4(2) . . ?
C1 C8 C7 116.1(2) . . ?
C1 C8 H8A 108.3 . . ?
C7 C8 H8A 108.3 . . ?
C1 C8 H8B 108.3 . . ?
C7 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
C7' C8 H8'A 109.1 . . ?
C1 C8 H8'A 109.1 . . ?
C7' C8 H8'B 109.1 . . ?
C1 C8 H8'B 109.1 . . ?
H8'A C8 H8'B 107.9 . . ?
C5 C4' C3 105.6(3) . . ?
C5 C4' H4'A 110.6 . . ?
C3 C4' H4'A 110.6 . . ?
C5 C4' H4'B 110.6 . . ?
C3 C4' H4'B 110.6 . . ?
H4'A C4' H4'B 108.7 . . ?
C8 C7' C6 113.4(3) . . ?
C8 C7' H7'A 108.9 . . ?
C6 C7' H7'A 108.9 . . ?
C8 C7' H7'B 108.9 . . ?
C6 C7' H7'B 108.9 . . ?
H7'A C7' H7'B 107.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh C6 2.0624(18) . ?
Rh C5 2.071(2) . ?
Rh N22 2.0920(15) . ?
Rh C2 2.1509(19) . ?
Rh C1 2.1552(19) . ?
Rh N12 2.2476(15) . ?
Rh N32 2.2628(15) . ?
N12 C13 1.333(2) . ?
N12 N11 1.356(2) . ?
N11 C15 1.343(2) . ?
N11 B1 1.531(2) . ?
C15 C14 1.379(3) . ?
C15 H15 0.95 . ?
C14 C13 1.398(3) . ?
C14 H14 0.95 . ?
C13 H13 0.95 . ?
N22 C23 1.330(2) . ?
N22 N21 1.358(2) . ?
N21 C25 1.345(2) . ?
N21 B1 1.543(2) . ?
C25 C24 1.374(3) . ?
C25 H25 0.95 . ?
C24 C23 1.386(3) . ?
C24 H24 0.95 . ?
C23 H23 0.95 . ?
N32 C33 1.334(2) . ?
N32 N31 1.360(2) . ?
N31 C35 1.350(2) . ?
N31 B1 1.528(2) . ?
C35 C34 1.376(3) . ?
C35 H35 0.95 . ?
C34 C33 1.397(3) . ?
C34 H34 0.95 . ?
C33 H33 0.95 . ?
B1 H1 1 . ?
C1 C2 1.381(3) . ?
C1 C8 1.502(3) . ?
C1 H1A 0.95 . ?
C2 C3 1.508(4) . ?
C2 H2 0.95 . ?
C3 C4 1.389(5) . ?
C3 C4' 1.619(5) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C3 H3'A 0.99 . ?
C3 H3'B 0.99 . ?
C4 C5 1.579(4) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C6 1.424(3) . ?
C5 C4' 1.512(4) . ?
C5 H5 0.95 . ?
C5 H5' 0.95 . ?
C6 C7' 1.530(4) . ?
C6 C7 1.559(4) . ?
C6 H6 0.95 . ?
C6 H6' 0.95 . ?
C7 C8 1.545(5) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 C7' 1.468(5) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C8 H8'A 0.99 . ?
C8 H8'B 0.99 . ?
C4' H4'A 0.99 . ?
C4' H4'B 0.99 . ?
C7' H7'A 0.99 . ?
C7' H7'B 0.99 . ?
