#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/49/7024973.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_7024973
loop_
_publ_author_name
'Seino, Hidetake'
'Misumi, Yoshiyuki'
'Hojo, Yoshihiro'
'Mizobe, Yasushi'
_publ_section_title
;
 Heterolytic H2 activation by rhodium thiolato complexes bearing the
 hydrotris(pyrazolyl)borato ligand and application to catalytic
 hydrogenation under mild conditions.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3072
_journal_page_last               3082
_journal_paper_doi               10.1039/b923557d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C21 H33 B I2 N7 O Rh '
_chemical_formula_sum            'C21 H33 B I2 N7 O Rh'
_chemical_formula_weight         767.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2009-08-09
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.916(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.9782(15)
_cell_length_b                   13.431(3)
_cell_length_c                   26.285(5)
_cell_measurement_reflns_used    8328
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      3.0
_cell_volume                     2789.7(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      113.1
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            33333
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.652
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1488.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.35
_refine_diff_density_min         -0.92
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6665
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.0019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0011Fo² + 1.0000σ(Fo²)]/(4Fo²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1166
_reflns_number_gt                5803
_reflns_number_total             6664
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b923557d.txt
_cod_data_source_block           '__[TpMe2RhI2(MeCN)]-THF'
_cod_original_cell_volume        2789.8(9)
_cod_original_formula_sum        'C21 H33 B I2 N7 O Rh '
_cod_database_code               7024973
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,1/2-Y,1/2+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
I(1) I 0.83277(4) 0.53564(3) 0.259160(10) 0.01855(8) Uani 1.00 1 d .
I(2) I 0.79053(4) 0.33399(2) 0.155690(10) 0.01881(8) Uani 1.00 1 d .
Rh(1) Rh 0.62380(4) 0.50027(3) 0.172440(10) 0.01134(8) Uani 1.00 1 d .
O(1) O 0.872(2) 0.1051(14) 0.0227(7) 0.102(6) Uani 0.50 1 d P
O(2) O 0.6743(13) -0.0034(8) 0.1028(4) 0.054(3) Uani 0.50 1 d P
N(1) N 0.4238(4) 0.5590(3) 0.07413(14) 0.0152(9) Uani 1.00 1 d .
N(2) N 0.4532(4) 0.4784(2) 0.10614(15) 0.0140(8) Uani 1.00 1 d .
N(3) N 0.4477(4) 0.6900(2) 0.14295(14) 0.0140(8) Uani 1.00 1 d .
N(4) N 0.4835(4) 0.6265(2) 0.18387(14) 0.0141(8) Uani 1.00 1 d .
N(5) N 0.6939(4) 0.6522(3) 0.09810(15) 0.0158(9) Uani 1.00 1 d .
N(6) N 0.7745(4) 0.5819(3) 0.13056(14) 0.0155(9) Uani 1.00 1 d .
N(7) N 0.4695(4) 0.4222(3) 0.21218(15) 0.0167(9) Uani 1.00 1 d .
C(1) C 0.3536(5) 0.4035(4) 0.08596(18) 0.0193(11) Uani 1.00 1 d .
C(2) C 0.2612(6) 0.4365(4) 0.03948(19) 0.0222(12) Uani 1.00 1 d .
C(3) C 0.3093(5) 0.5337(4) 0.03303(18) 0.0200(11) Uani 1.00 1 d .
C(4) C 0.3361(6) 0.3041(4) 0.1102(2) 0.0276(13) Uani 1.00 1 d .
C(5) C 0.2548(6) 0.6032(4) -0.01025(19) 0.0279(13) Uani 1.00 1 d .
C(6) C 0.4051(5) 0.6634(3) 0.22256(18) 0.0162(10) Uani 1.00 1 d .
C(7) C 0.3230(5) 0.7515(3) 0.20574(18) 0.0190(11) Uani 1.00 1 d .
C(8) C 0.3517(5) 0.7667(3) 0.15609(18) 0.0176(11) Uani 1.00 1 d .
C(9) C 0.4041(6) 0.6147(4) 0.27349(18) 0.0240(12) Uani 1.00 1 d .
C(10) C 0.3005(6) 0.8529(3) 0.1209(2) 0.0245(12) Uani 1.00 1 d .
C(11) C 0.9418(5) 0.5907(3) 0.12724(18) 0.0179(11) Uani 1.00 1 d .
C(12) C 0.9638(6) 0.6646(3) 0.09215(19) 0.0204(11) Uani 1.00 1 d .
C(13) C 0.8082(6) 0.7028(3) 0.07450(18) 0.0188(11) Uani 1.00 1 d .
C(14) C 1.0799(6) 0.5291(4) 0.1552(2) 0.0290(14) Uani 1.00 1 d .
C(15) C 0.7591(7) 0.7854(4) 0.0376(2) 0.0302(14) Uani 1.00 1 d .
C(16) C 0.3766(6) 0.3832(3) 0.23409(19) 0.0206(11) Uani 1.00 1 d .
C(17) C 0.2548(6) 0.3345(4) 0.2622(2) 0.0310(14) Uani 1.00 1 d .
C(18) C 0.974(3) 0.104(2) 0.0695(11) 0.093(9) Uani 0.50 1 d P
C(19) C 0.8571(14) 0.0384(12) 0.1088(5) 0.115(5) Uani 1.00 1 d .
C(20) C 0.682(2) 0.070(2) 0.0759(7) 0.065(6) Uani 0.50 1 d P
C(21) C 0.717(3) 0.0787(18) 0.0212(9) 0.075(8) Uani 0.50 1 d P
C(22) C 0.894(5) 0.074(2) 0.0675(12) 0.130(13) Uani 0.50 1 d P
C(23) C 0.678(3) 0.110(2) 0.0431(13) 0.090(10) Uani 0.50 1 d P
C(24) C 0.589(3) 0.072(2) 0.0773(11) 0.092(9) Uani 0.50 1 d P
B(1) B 0.5009(6) 0.6607(3) 0.0906(2) 0.0147(11) Uani 1.00 1 d .
H(1) H 0.473(6) 0.713(4) 0.063(2) 0.0184 Uiso 1.00 1 c .
H(2) H 0.1815 0.3990 0.0171 0.026 Uiso 1.00 1 c R
H(3) H 0.4174 0.2594 0.0999 0.033 Uiso 1.00 1 c R
H(4) H 0.2256 0.2786 0.0998 0.033 Uiso 1.00 1 c R
H(5) H 0.3543 0.3112 0.1465 0.033 Uiso 1.00 1 c R
H(6) H 0.1594 0.6403 -0.0031 0.033 Uiso 1.00 1 c R
H(7) H 0.2255 0.5663 -0.0410 0.033 Uiso 1.00 1 c R
H(8) H 0.3450 0.6474 -0.0142 0.033 Uiso 1.00 1 c R
H(9) H 0.2586 0.7931 0.2250 0.023 Uiso 1.00 1 c R
H(10) H 0.3090 0.5717 0.2719 0.029 Uiso 1.00 1 c R
H(11) H 0.3972 0.6643 0.2989 0.029 Uiso 1.00 1 c R
H(12) H 0.5050 0.5772 0.2821 0.029 Uiso 1.00 1 c R
H(13) H 0.3835 0.9039 0.1264 0.029 Uiso 1.00 1 c R
H(14) H 0.1945 0.8782 0.1276 0.030 Uiso 1.00 1 c R
H(15) H 0.2909 0.8309 0.0863 0.029 Uiso 1.00 1 c R
H(16) H 1.0683 0.6851 0.0821 0.025 Uiso 1.00 1 c R
H(17) H 1.1199 0.5595 0.1872 0.035 Uiso 1.00 1 c R
H(18) H 1.1700 0.5240 0.1352 0.035 Uiso 1.00 1 c R
H(19) H 1.0380 0.4644 0.1611 0.035 Uiso 1.00 1 c R
H(20) H 0.7354 0.7593 0.0038 0.037 Uiso 1.00 1 c R
H(21) H 0.8499 0.8315 0.0391 0.037 Uiso 1.00 1 c R
H(22) H 0.6615 0.8182 0.0464 0.037 Uiso 1.00 1 c R
H(23) H 0.2836 0.3476 0.2979 0.039 Uiso 1.00 1 c R
H(24) H 0.2571 0.2648 0.2564 0.039 Uiso 1.00 1 c R
H(25) H 0.1445 0.3594 0.2509 0.039 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
B B 0.001 0.001
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.474 1.812
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Rh Rh -1.118 0.919
;
International Tables for Crystallography
(1992, 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_publ_flag
I(1) Rh(1) I(2) 91.312(13) yes
I(1) Rh(1) N(2) 177.08(11) yes
I(1) Rh(1) N(4) 90.96(9) yes
I(1) Rh(1) N(6) 91.13(9) yes
I(1) Rh(1) N(7) 90.24(10) yes
I(2) Rh(1) N(2) 91.54(10) yes
I(2) Rh(1) N(4) 177.28(9) yes
I(2) Rh(1) N(6) 90.96(11) yes
I(2) Rh(1) N(7) 90.24(11) yes
N(2) Rh(1) N(4) 86.16(14) yes
N(2) Rh(1) N(6) 89.45(14) yes
N(2) Rh(1) N(7) 89.13(15) yes
N(4) Rh(1) N(6) 90.49(15) yes
N(4) Rh(1) N(7) 88.27(15) yes
N(6) Rh(1) N(7) 178.16(14) yes
C(18) O(1) C(21) 118(2) yes
C(19) O(2) C(24) 100.3(14) yes
N(2) N(1) C(3) 109.3(3) yes
N(2) N(1) B(1) 120.1(3) yes
C(3) N(1) B(1) 130.2(4) yes
Rh(1) N(2) N(1) 116.1(2) yes
Rh(1) N(2) C(1) 136.0(3) yes
N(1) N(2) C(1) 107.9(3) yes
N(4) N(3) C(8) 109.7(3) yes
N(4) N(3) B(1) 119.1(3) yes
C(8) N(3) B(1) 130.8(3) yes
Rh(1) N(4) N(3) 116.9(2) yes
Rh(1) N(4) C(6) 136.0(3) yes
N(3) N(4) C(6) 107.0(3) yes
N(6) N(5) C(13) 110.1(3) yes
N(6) N(5) B(1) 120.6(3) yes
C(13) N(5) B(1) 129.2(3) yes
Rh(1) N(6) N(5) 116.2(2) yes
Rh(1) N(6) C(11) 137.3(3) yes
N(5) N(6) C(11) 106.4(3) yes
Rh(1) N(7) C(16) 175.9(4) yes
N(2) C(1) C(2) 108.4(4) yes
N(2) C(1) C(4) 125.8(4) yes
C(2) C(1) C(4) 125.7(4) yes
C(1) C(2) C(3) 106.5(4) yes
N(1) C(3) C(2) 107.9(4) yes
N(1) C(3) C(5) 123.0(4) yes
C(2) C(3) C(5) 129.1(4) yes
N(4) C(6) C(7) 108.5(4) yes
N(4) C(6) C(9) 124.8(4) yes
C(7) C(6) C(9) 126.6(4) yes
C(6) C(7) C(8) 107.1(4) yes
N(3) C(8) C(7) 107.7(4) yes
N(3) C(8) C(10) 122.9(4) yes
C(7) C(8) C(10) 129.3(4) yes
N(6) C(11) C(12) 108.8(3) yes
N(6) C(11) C(14) 126.1(4) yes
C(12) C(11) C(14) 125.2(4) yes
C(11) C(12) C(13) 107.7(4) yes
N(5) C(13) C(12) 107.1(4) yes
N(5) C(13) C(15) 122.6(4) yes
C(12) C(13) C(15) 130.3(4) yes
N(7) C(16) C(17) 178.9(5) yes
O(1) C(18) C(19) 103.7(18) yes
O(2) C(19) C(22) 112.3(19) yes
C(18) C(19) C(20) 92.5(14) yes
C(19) C(20) C(21) 105.7(18) yes
O(1) C(21) C(20) 107(2) yes
C(19) C(22) C(23) 95(2) yes
C(22) C(23) C(24) 103(2) yes
O(2) C(24) C(23) 110(2) yes
N(1) B(1) N(3) 109.2(3) yes
N(1) B(1) N(5) 109.0(3) yes
N(3) B(1) N(5) 107.4(3) yes
C(1) C(2) H(2) 126.6 no
C(3) C(2) H(2) 126.9 no
C(1) C(4) H(3) 109.6 no
C(1) C(4) H(4) 109.7 no
C(1) C(4) H(5) 109.1 no
H(3) C(4) H(4) 109.5 no
H(3) C(4) H(5) 109.5 no
H(4) C(4) H(5) 109.5 no
C(3) C(5) H(6) 109.6 no
C(3) C(5) H(7) 109.6 no
C(3) C(5) H(8) 109.3 no
H(6) C(5) H(7) 109.5 no
H(6) C(5) H(8) 109.5 no
H(7) C(5) H(8) 109.5 no
C(6) C(7) H(9) 126.4 no
C(8) C(7) H(9) 126.4 no
C(6) C(9) H(10) 109.4 no
C(6) C(9) H(11) 109.3 no
C(6) C(9) H(12) 109.8 no
H(10) C(9) H(11) 109.5 no
H(10) C(9) H(12) 109.5 no
H(11) C(9) H(12) 109.5 no
C(8) C(10) H(13) 109.7 no
C(8) C(10) H(14) 109.5 no
C(8) C(10) H(15) 109.2 no
H(13) C(10) H(14) 109.5 no
H(13) C(10) H(15) 109.5 no
H(14) C(10) H(15) 109.5 no
C(11) C(12) H(16) 126.2 no
C(13) C(12) H(16) 126.1 no
C(11) C(14) H(17) 109.5 no
C(11) C(14) H(18) 109.3 no
C(11) C(14) H(19) 109.6 no
H(17) C(14) H(18) 109.5 no
H(17) C(14) H(19) 109.5 no
H(18) C(14) H(19) 109.5 no
C(13) C(15) H(20) 109.6 no
C(13) C(15) H(21) 109.1 no
C(13) C(15) H(22) 109.7 no
H(20) C(15) H(21) 109.5 no
H(20) C(15) H(22) 109.5 no
H(21) C(15) H(22) 109.5 no
C(16) C(17) H(23) 109.3 no
C(16) C(17) H(24) 109.4 no
C(16) C(17) H(25) 109.7 no
H(23) C(17) H(24) 109.5 no
H(23) C(17) H(25) 109.5 no
H(24) C(17) H(25) 109.5 no
N(1) B(1) H(1) 112(3) no
N(3) B(1) H(1) 114(3) no
N(5) B(1) H(1) 105(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
I(1) Rh(1) 2.6747(3) yes
I(2) Rh(1) 2.6669(4) yes
Rh(1) N(2) 2.079(3) yes
Rh(1) N(4) 2.076(3) yes
Rh(1) N(6) 2.055(4) yes
Rh(1) N(7) 2.015(4) yes
O(1) C(18) 1.38(3) yes
O(1) C(21) 1.28(3) yes
O(2) C(19) 1.551(16) yes
O(2) C(24) 1.35(3) yes
N(1) N(2) 1.372(5) yes
N(1) C(3) 1.358(5) yes
N(1) B(1) 1.536(6) yes
N(2) C(1) 1.345(6) yes
N(3) N(4) 1.372(5) yes
N(3) C(8) 1.356(6) yes
N(3) B(1) 1.546(6) yes
N(4) C(6) 1.359(6) yes
N(5) N(6) 1.371(5) yes
N(5) C(13) 1.355(6) yes
N(5) B(1) 1.530(6) yes
N(6) C(11) 1.355(5) yes
N(7) C(16) 1.129(6) yes
C(1) C(2) 1.409(6) yes
C(1) C(4) 1.494(7) yes
C(2) C(3) 1.377(7) yes
C(3) C(5) 1.489(7) yes
C(6) C(7) 1.395(6) yes
C(6) C(9) 1.491(6) yes
C(7) C(8) 1.371(6) yes
C(8) C(10) 1.503(6) yes
C(11) C(12) 1.383(7) yes
C(11) C(14) 1.489(6) yes
C(12) C(13) 1.364(6) yes
C(13) C(15) 1.490(7) yes
C(16) C(17) 1.455(8) yes
C(18) C(19) 1.73(3) yes
C(19) C(20) 1.60(2) yes
C(19) C(22) 1.26(3) yes
C(20) C(21) 1.51(3) yes
C(22) C(23) 1.81(4) yes
C(23) C(24) 1.32(4) yes
C(2) H(2) 0.950 no
C(4) H(3) 0.950 no
C(4) H(4) 0.950 no
C(4) H(5) 0.950 no
C(5) H(6) 0.950 no
C(5) H(7) 0.950 no
C(5) H(8) 0.950 no
C(7) H(9) 0.950 no
C(9) H(10) 0.950 no
C(9) H(11) 0.950 no
C(9) H(12) 0.950 no
C(10) H(13) 0.950 no
C(10) H(14) 0.950 no
C(10) H(15) 0.950 no
C(12) H(16) 0.950 no
C(14) H(17) 0.950 no
C(14) H(18) 0.950 no
C(14) H(19) 0.950 no
C(15) H(20) 0.950 no
C(15) H(21) 0.950 no
C(15) H(22) 0.950 no
C(17) H(23) 0.950 no
C(17) H(24) 0.950 no
C(17) H(25) 0.950 no
B(1) H(1) 1.01(5) no
