# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011


data_publication_text
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
#TrackingRef '1.CIF'

_publ_contact_author_name        'Richard A. Jones'
_publ_contact_author_address     
;Department of Chemistry and Biochemistry
The University of Texas at Austin
1 University Station A5300
Austin, Texas, 78712-0165
;
_publ_contact_author_email       rajones@mail.utexas.edu
_publ_contact_author_phone       '(512) 471-1706'
loop_
_publ_author_name
_publ_author_address
W.J.McCarty
;Department of Chemistry and Biochemistry
The University of Texas at Austin
1 University Station A5300
Austin, Texas, 78712-0165
;
'Xiaoping Yang'
;Department of Chemistry and Biochemistry
The University of Texas at Austin
1 University Station A5300
Austin, Texas, 78712-0165
;
'Richard A. Jones'
;Department of Chemistry and Biochemistry
The University of Texas at Austin
1 University Station A5300
Austin, Texas, 78712-0165
;

data_Complex-1
_database_code_depnum_ccdc_archive 'CCDC 772323'
#TrackingRef '1.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
;
Dilithium (tetrakis(3,5-
bis(trifluoromethyl)pyrazolato))rhodium(ii) di-tetrahydrofuran disolvate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H20 F24 Li2 N8 O2 Rh1'
_chemical_formula_sum            'C28 H20 F24 Li2 N8 O2 Rh'
_chemical_formula_weight         1073.31

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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
O O 0.0106 0.0060 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.439(2)
_cell_length_b                   9.2437(18)
_cell_length_c                   19.437(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.65(3)
_cell_angle_gamma                90.00
_cell_volume                     1969.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    4100
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1054
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.9016
_exptl_absorpt_correction_T_max  0.9436
_exptl_absorpt_process_details   
;
Absorption correction given as Gaussian
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6382
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3460
_reflns_number_gt                2834
_reflns_threshold_expression     >2sigma(I)

_publ_section_references         
;
Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97.
(1999) J. Appl. Cryst. 32, 115-119.

Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838.

Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology,
276, Macromolecular Crystallography, part A, 307-326, C. W. Carter,
Jr. and R. M. Sweets, Eds., Academic Press.

Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens
Analytical X-ray Instruments, Inc., Madison, WI, USA.

Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201.

Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht
University, Utrecht, The Netherlands.

;

_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_reduction        
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+2.4061P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3460
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0882
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Rh1 Rh 0.5000 0.0000 0.0000 0.02362(13) Uani 1 2 d SU . .
Li1 Li 0.3135(5) -0.2313(8) 0.0619(3) 0.0430(15) Uani 1 1 d U . .
O1 O 0.2455(2) -0.2005(3) 0.13694(13) 0.0517(7) Uani 1 1 d U . .
N1 N 0.6515(2) 0.0942(3) 0.06703(13) 0.0266(6) Uani 1 1 d U . .
N2 N 0.7315(2) 0.1652(3) 0.03992(14) 0.0296(6) Uani 1 1 d U . .
N3 N 0.4887(2) -0.2778(3) 0.07197(13) 0.0286(6) Uani 1 1 d U . .
N4 N 0.5599(2) -0.1983(3) 0.04106(13) 0.0274(6) Uani 1 1 d U . .
F1 F 0.6464(3) 0.1008(3) 0.24800(12) 0.0665(7) Uani 1 1 d U . .
F2 F 0.5044(2) 0.0305(3) 0.15486(12) 0.0511(6) Uani 1 1 d U . .
F3 F 0.6564(2) -0.1072(3) 0.20160(12) 0.0576(6) Uani 1 1 d U . .
F4 F 0.9667(3) 0.3956(4) 0.13258(15) 0.0857(10) Uani 1 1 d U . .
F5 F 1.0208(2) 0.2063(3) 0.0869(2) 0.0898(10) Uani 1 1 d U . .
F6 F 0.8983(2) 0.3554(3) 0.02034(13) 0.0607(7) Uani 1 1 d U . .
F7 F 0.5138(2) -0.6455(2) 0.11325(14) 0.0606(7) Uani 1 1 d U . .
F8 F 0.5342(3) -0.5016(3) 0.20155(12) 0.0765(9) Uani 1 1 d U . .
F9 F 0.3719(2) -0.4967(3) 0.11350(14) 0.0586(6) Uani 1 1 d U . .
F10 F 0.8223(2) -0.3292(3) -0.00199(14) 0.0621(7) Uani 1 1 d U . .
F11 F 0.7144(2) -0.1406(3) -0.04498(12) 0.0537(6) Uani 1 1 d U . .
F12 F 0.83987(19) -0.1355(3) 0.06053(13) 0.0547(6) Uani 1 1 d U . .
C1 C 0.6258(4) 0.0319(4) 0.18565(19) 0.0418(9) Uani 1 1 d U . .
C2 C 0.6931(3) 0.0979(4) 0.13950(17) 0.0304(8) Uani 1 1 d U . .
C3 C 0.8018(3) 0.1724(4) 0.16055(18) 0.0352(8) Uani 1 1 d U . .
H3A H 0.8499 0.1918 0.2070 0.042 Uiso 1 1 calc R . .
C4 C 0.8222(3) 0.2115(4) 0.09663(18) 0.0330(8) Uani 1 1 d U . .
C5 C 0.9266(3) 0.2906(5) 0.0840(2) 0.0452(10) Uani 1 1 d U . .
C6 C 0.4939(4) -0.5106(4) 0.13053(19) 0.0393(9) Uani 1 1 d U . .
C7 C 0.5489(3) -0.4018(4) 0.09377(17) 0.0315(8) Uani 1 1 d U . .
C8 C 0.6587(3) -0.4056(4) 0.07750(18) 0.0369(8) Uani 1 1 d U . .
H8A H 0.7167 -0.4791 0.0868 0.044 Uiso 1 1 calc R . .
C9 C 0.6618(3) -0.2746(4) 0.04422(17) 0.0317(8) Uani 1 1 d U . .
C10 C 0.7589(3) -0.2204(4) 0.0146(2) 0.0416(9) Uani 1 1 d U . .
C11 C 0.1227(5) -0.1674(9) 0.1270(3) 0.113(2) Uani 1 1 d DU . .
H11A H 0.0716 -0.2326 0.0919 0.136 Uiso 1 1 calc R . .
H11B H 0.1061 -0.0692 0.1093 0.136 Uiso 1 1 calc R . .
C12 C 0.0963(6) -0.1822(12) 0.1950(3) 0.115(3) Uani 1 1 d DU . .
H12A H 0.0420 -0.2635 0.1935 0.138 Uiso 1 1 calc R . .
H12B H 0.0572 -0.0953 0.2056 0.138 Uiso 1 1 calc R . .
C13 C 0.2121(5) -0.2058(9) 0.2499(3) 0.104(2) Uani 1 1 d DU . .
H13A H 0.2119 -0.2986 0.2731 0.125 Uiso 1 1 calc R . .
H13B H 0.2263 -0.1304 0.2860 0.125 Uiso 1 1 calc R . .
C14 C 0.3060(5) -0.2024(7) 0.2126(2) 0.0813(17) Uani 1 1 d U . .
H14A H 0.3563 -0.1168 0.2263 0.098 Uiso 1 1 calc R . .
H14B H 0.3579 -0.2871 0.2249 0.098 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.02094(19) 0.0266(2) 0.02198(19) 0.00203(15) 0.00393(13) 0.00098(16)
Li1 0.033(3) 0.061(4) 0.038(3) 0.011(3) 0.014(2) 0.003(3)
O1 0.0362(14) 0.081(2) 0.0408(14) 0.0097(14) 0.0166(12) 0.0148(14)
N1 0.0241(14) 0.0277(15) 0.0256(13) 0.0021(12) 0.0035(11) 0.0001(12)
N2 0.0255(14) 0.0312(16) 0.0304(14) 0.0017(12) 0.0050(12) 0.0006(12)
N3 0.0283(14) 0.0304(15) 0.0262(14) 0.0022(12) 0.0061(11) -0.0011(12)
N4 0.0242(14) 0.0288(15) 0.0273(14) 0.0020(12) 0.0044(11) 0.0030(12)
F1 0.0896(19) 0.0804(18) 0.0363(12) -0.0148(13) 0.0289(12) -0.0238(15)
F2 0.0422(13) 0.0637(15) 0.0509(13) 0.0091(11) 0.0188(10) -0.0048(11)
F3 0.0744(17) 0.0505(15) 0.0452(13) 0.0199(11) 0.0129(11) 0.0007(13)
F4 0.0775(19) 0.099(2) 0.0775(18) -0.0270(17) 0.0177(15) -0.0573(18)
F5 0.0387(14) 0.082(2) 0.157(3) 0.040(2) 0.0416(16) 0.0142(14)
F6 0.0536(15) 0.0655(16) 0.0621(15) 0.0175(13) 0.0151(12) -0.0134(13)
F7 0.0790(18) 0.0306(12) 0.0761(17) 0.0075(12) 0.0286(14) 0.0008(12)
F8 0.115(2) 0.0757(18) 0.0322(12) 0.0068(12) 0.0106(13) -0.0434(17)
F9 0.0501(14) 0.0546(15) 0.0775(17) 0.0168(13) 0.0284(12) -0.0018(12)
F10 0.0535(15) 0.0517(15) 0.0959(19) -0.0037(14) 0.0451(14) 0.0069(12)
F11 0.0462(13) 0.0649(16) 0.0542(13) 0.0152(12) 0.0210(11) -0.0023(12)
F12 0.0275(11) 0.0560(15) 0.0765(16) -0.0059(13) 0.0083(11) -0.0043(11)
C1 0.046(2) 0.049(2) 0.0292(18) 0.0008(17) 0.0085(16) -0.0025(18)
C2 0.0332(18) 0.0291(18) 0.0264(17) 0.0006(14) 0.0048(14) 0.0047(15)
C3 0.0349(19) 0.036(2) 0.0286(17) -0.0014(15) -0.0008(14) 0.0013(16)
C4 0.0263(17) 0.0327(19) 0.0360(19) -0.0007(15) 0.0025(14) 0.0007(15)
C5 0.032(2) 0.048(2) 0.051(2) 0.000(2) 0.0038(17) -0.0040(19)
C6 0.047(2) 0.033(2) 0.0349(19) 0.0035(16) 0.0077(16) -0.0012(18)
C7 0.0339(19) 0.0296(18) 0.0271(16) 0.0018(15) 0.0022(14) -0.0018(15)
C8 0.0323(19) 0.035(2) 0.041(2) 0.0021(16) 0.0056(15) 0.0069(16)
C9 0.0270(17) 0.0338(19) 0.0314(17) 0.0002(15) 0.0036(14) 0.0025(15)
C10 0.0328(19) 0.040(2) 0.053(2) 0.0019(19) 0.0151(17) 0.0061(18)
C11 0.062(3) 0.195(7) 0.089(4) -0.002(4) 0.031(3) 0.041(4)
C12 0.079(4) 0.190(9) 0.093(4) -0.033(5) 0.051(4) 0.000(5)
C13 0.099(4) 0.157(6) 0.071(3) 0.007(4) 0.046(3) 0.021(4)
C14 0.071(3) 0.127(5) 0.050(3) -0.003(3) 0.023(2) 0.015(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Rh1 N4 2.037(3) 3_655 ?
Rh1 N4 2.037(3) . ?
Rh1 N1 2.041(3) . ?
Rh1 N1 2.041(3) 3_655 ?
Li1 O1 1.860(7) . ?
Li1 N2 1.993(6) 3_655 ?
Li1 N3 2.004(7) . ?
O1 C11 1.396(6) . ?
O1 C14 1.434(5) . ?
N1 N2 1.350(4) . ?
N1 C2 1.352(4) . ?
N2 C4 1.349(4) . ?
N2 Li1 1.993(6) 3_655 ?
N3 C7 1.342(4) . ?
N3 N4 1.358(4) . ?
N4 C9 1.349(4) . ?
F1 C1 1.329(4) . ?
F2 C1 1.346(4) . ?
F3 C1 1.345(4) . ?
F4 C5 1.340(5) . ?
F5 C5 1.318(5) . ?
F6 C5 1.329(4) . ?
F7 C6 1.328(4) . ?
F8 C6 1.327(4) . ?
F9 C6 1.344(5) . ?
F10 C10 1.332(4) . ?
F11 C10 1.344(4) . ?
F12 C10 1.340(4) . ?
C1 C2 1.471(5) . ?
C2 C3 1.377(5) . ?
C3 C4 1.377(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.479(5) . ?
C6 C7 1.475(5) . ?
C7 C8 1.381(5) . ?
C8 C9 1.378(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.478(5) . ?
C11 C12 1.445(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.459(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.458(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?

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
N4 Rh1 N4 180.0(2) 3_655 . ?
N4 Rh1 N1 89.71(10) 3_655 . ?
N4 Rh1 N1 90.29(10) . . ?
N4 Rh1 N1 90.29(10) 3_655 3_655 ?
N4 Rh1 N1 89.71(10) . 3_655 ?
N1 Rh1 N1 180.00(19) . 3_655 ?
O1 Li1 N2 133.2(4) . 3_655 ?
O1 Li1 N3 126.0(3) . . ?
N2 Li1 N3 97.4(3) 3_655 . ?
C11 O1 C14 108.4(4) . . ?
C11 O1 Li1 123.7(3) . . ?
C14 O1 Li1 127.9(3) . . ?
N2 N1 C2 108.6(3) . . ?
N2 N1 Rh1 120.33(19) . . ?
C2 N1 Rh1 131.0(2) . . ?
C4 N2 N1 106.5(3) . . ?
C4 N2 Li1 129.4(3) . 3_655 ?
N1 N2 Li1 121.7(3) . 3_655 ?
C7 N3 N4 106.5(3) . . ?
C7 N3 Li1 128.5(3) . . ?
N4 N3 Li1 123.4(3) . . ?
C9 N4 N3 108.5(3) . . ?
C9 N4 Rh1 132.6(2) . . ?
N3 N4 Rh1 118.9(2) . . ?
F1 C1 F3 106.3(3) . . ?
F1 C1 F2 107.5(3) . . ?
F3 C1 F2 105.1(3) . . ?
F1 C1 C2 111.7(3) . . ?
F3 C1 C2 113.0(3) . . ?
F2 C1 C2 112.7(3) . . ?
N1 C2 C3 109.9(3) . . ?
N1 C2 C1 122.4(3) . . ?
C3 C2 C1 127.7(3) . . ?
C4 C3 C2 103.6(3) . . ?
C4 C3 H3A 128.2 . . ?
C2 C3 H3A 128.2 . . ?
N2 C4 C3 111.4(3) . . ?
N2 C4 C5 119.3(3) . . ?
C3 C4 C5 129.3(3) . . ?
F5 C5 F6 106.5(3) . . ?
F5 C5 F4 106.7(3) . . ?
F6 C5 F4 105.8(3) . . ?
F5 C5 C4 112.9(3) . . ?
F6 C5 C4 112.6(3) . . ?
F4 C5 C4 111.8(3) . . ?
F8 C6 F7 106.8(3) . . ?
F8 C6 F9 106.1(3) . . ?
F7 C6 F9 105.6(3) . . ?
F8 C6 C7 113.1(3) . . ?
F7 C6 C7 112.9(3) . . ?
F9 C6 C7 111.9(3) . . ?
N3 C7 C8 111.6(3) . . ?
N3 C7 C6 118.9(3) . . ?
C8 C7 C6 129.5(3) . . ?
C9 C8 C7 103.4(3) . . ?
C9 C8 H8A 128.3 . . ?
C7 C8 H8A 128.3 . . ?
N4 C9 C8 110.1(3) . . ?
N4 C9 C10 122.8(3) . . ?
C8 C9 C10 127.2(3) . . ?
F10 C10 F12 106.5(3) . . ?
F10 C10 F11 107.7(3) . . ?
F12 C10 F11 105.7(3) . . ?
F10 C10 C9 111.1(3) . . ?
F12 C10 C9 113.1(3) . . ?
F11 C10 C9 112.4(3) . . ?
O1 C11 C12 108.5(5) . . ?
O1 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
O1 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
C11 C12 C13 107.4(5) . . ?
C11 C12 H12A 110.2 . . ?
C13 C12 H12A 110.2 . . ?
C11 C12 H12B 110.2 . . ?
C13 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
C12 C13 C14 106.1(4) . . ?
C12 C13 H13A 110.5 . . ?
C14 C13 H13A 110.5 . . ?
C12 C13 H13B 110.5 . . ?
C14 C13 H13B 110.5 . . ?
H13A C13 H13B 108.7 . . ?
O1 C14 C13 107.6(4) . . ?
O1 C14 H14A 110.2 . . ?
C13 C14 H14A 110.2 . . ?
O1 C14 H14B 110.2 . . ?
C13 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.067