# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013
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#
# Cambridge Crystallographic Data Centre
# CCDC
#
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#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
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data_kcd129
_database_code_depnum_ccdc_archive 'CCDC 809638'
#TrackingRef 'CCDC_809638-809639.cif'
_database_code_depnum_ccdc_archive 'CCDC 809638'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
rac-\D*-bis(ethane-1,2-diamine)[(S*)-N-methyl-3-nitro-(R*)-
alaninato-\k^2^N,O^1^]cobalt(III) tetrachloridozincate
;
_chemical_name_common
;
rac-cdelta*-bis(ethane-1,2-diamine)((S*)-N-methyl-3-nitro-
(R*)-alaninato-kappa$2!N,O$1!)cobalt(iii) tetrachloridozincate
;
_chemical_melting_point ?
_chemical_formula_moiety 'C8 H23 Co N6 O4, Cl4 Zn'
_chemical_formula_sum 'C8 H23 Cl4 Co N6 O4 Zn'
_chemical_formula_weight 533.42
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C c'
_symmetry_space_group_name_Hall 'C -2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
_cell_length_a 9.739(2)
_cell_length_b 17.035(3)
_cell_length_c 11.652(6)
_cell_angle_alpha 90.00
_cell_angle_beta 103.84(3)
_cell_angle_gamma 90.00
_cell_volume 1876.9(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 122(1)
_cell_measurement_reflns_used 25110
_cell_measurement_theta_min 2.39
_cell_measurement_theta_max 33.00
_exptl_crystal_description prism
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.03
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.888
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1080
_exptl_absorpt_coefficient_mu 2.757
_exptl_absorpt_correction_type integration
_exptl_absorpt_correction_T_min 0.215
_exptl_absorpt_correction_T_max 0.852
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 122(1)
_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 'Nonius KappaCCD area-detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_reflns_number 62337
_diffrn_reflns_av_R_equivalents 0.1036
_diffrn_reflns_av_sigmaI/netI 0.0356
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 2.39
_diffrn_reflns_theta_max 33.00
_reflns_number_total 6997
_reflns_number_gt 6573
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'COLLECT (Nonius, 1999)'
_computing_cell_refinement 'COLLECT (Nonius, 1999)'
_computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics
;
Ortep-3 (Farrugia, 1997) and Mercury (Macrae et. al., 2006)
;
_computing_publication_material SHELXL-97
_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^)+(0.0570P)^2^+6.0734P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.004(11)
_refine_ls_number_reflns 6997
_refine_ls_number_parameters 217
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0475
_refine_ls_R_factor_gt 0.0411
_refine_ls_wR_factor_ref 0.1094
_refine_ls_wR_factor_gt 0.1028
_refine_ls_goodness_of_fit_ref 1.120
_refine_ls_restrained_S_all 1.120
_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
Co Co -0.18064(4) 0.18464(2) -0.20298(4) 0.01192(8) Uani 1 1 d . . .
N1 N -0.0257(3) 0.13055(18) -0.2551(2) 0.0159(5) Uani 1 1 d . . .
H1 H -0.0506 0.0760 -0.2550 0.019 Uiso 1 1 d R . .
N2 N -0.2495(3) 0.08411(17) -0.1533(3) 0.0185(5) Uani 1 1 d . . .
H2A H -0.1845 0.0451 -0.1548 0.022 Uiso 1 1 calc R . .
H2B H -0.2602 0.0884 -0.0772 0.022 Uiso 1 1 calc R . .
N3 N -0.3256(3) 0.16980(16) -0.3508(2) 0.0146(4) Uani 1 1 d . . .
H3A H -0.3991 0.2042 -0.3534 0.018 Uiso 1 1 calc R . .
H3B H -0.2876 0.1801 -0.4143 0.018 Uiso 1 1 calc R . .
N4 N -0.3125(3) 0.24231(17) -0.1316(3) 0.0171(5) Uani 1 1 d . . .
H4A H -0.4003 0.2191 -0.1521 0.020 Uiso 1 1 calc R . .
H4B H -0.2816 0.2410 -0.0505 0.020 Uiso 1 1 calc R . .
N5 N -0.1248(3) 0.28792(16) -0.2502(2) 0.0142(4) Uani 1 1 d . . .
H5A H -0.0279 0.2908 -0.2362 0.017 Uiso 1 1 calc R . .
H5B H -0.1622 0.2955 -0.3298 0.017 Uiso 1 1 calc R . .
O1 O -0.0490(3) 0.19582(15) -0.0563(2) 0.0178(4) Uani 1 1 d . . .
O2 O 0.1737(3) 0.17353(19) 0.0391(2) 0.0264(6) Uani 1 1 d . . .
N13 N 0.1810(4) 0.0185(2) -0.0627(3) 0.0281(7) Uani 1 1 d . . .
O3 O 0.0572(4) 0.0087(2) -0.0607(3) 0.0342(7) Uani 1 1 d . . .
O4 O 0.2790(4) -0.0203(2) -0.0044(4) 0.0445(9) Uani 1 1 d . . .
C10 C -0.0104(4) 0.1408(2) -0.3777(3) 0.0188(6) Uani 1 1 d . . .
H10A H 0.0708 0.1102 -0.3886 0.023 Uiso 1 1 calc R . .
H10B H 0.0047 0.1964 -0.3922 0.023 Uiso 1 1 calc R . .
H10C H -0.0964 0.1224 -0.4334 0.023 Uiso 1 1 calc R . .
C11 C 0.1052(3) 0.1441(2) -0.1668(3) 0.0176(5) Uani 1 1 d . . .
H11 H 0.1495 0.1902 -0.1969 0.021 Uiso 1 1 calc R . .
C12 C 0.0763(4) 0.1718(2) -0.0508(3) 0.0173(5) Uani 1 1 d . . .
C13 C 0.2164(4) 0.0813(2) -0.1478(4) 0.0267(7) Uani 1 1 d . . .
H13A H 0.3104 0.1045 -0.1133 0.032 Uiso 1 1 calc R . .
H13B H 0.2189 0.0567 -0.2243 0.032 Uiso 1 1 calc R . .
C21 C -0.3871(4) 0.0635(2) -0.2342(3) 0.0191(6) Uani 1 1 d . . .
H21A H -0.4651 0.0918 -0.2110 0.023 Uiso 1 1 calc R . .
H21B H -0.4047 0.0064 -0.2310 0.023 Uiso 1 1 calc R . .
C31 C -0.3794(4) 0.08719(19) -0.3580(3) 0.0181(5) Uani 1 1 d . . .
H31A H -0.3145 0.0519 -0.3873 0.022 Uiso 1 1 calc R . .
H31B H -0.4742 0.0840 -0.4127 0.022 Uiso 1 1 calc R . .
C41 C -0.3225(4) 0.3249(2) -0.1733(4) 0.0222(6) Uani 1 1 d . . .
H41A H -0.3559 0.3591 -0.1169 0.027 Uiso 1 1 calc R . .
H41B H -0.3898 0.3291 -0.2515 0.027 Uiso 1 1 calc R . .
C51 C -0.1776(4) 0.3490(2) -0.1817(4) 0.0246(7) Uani 1 1 d . . .
H51A H -0.1813 0.4005 -0.2218 0.030 Uiso 1 1 calc R . .
H51B H -0.1142 0.3537 -0.1017 0.030 Uiso 1 1 calc R . .
Zn1 Zn -0.23468(4) -0.14960(2) -0.30371(3) 0.01551(8) Uani 1 1 d . . .
Cl1 Cl -0.08810(10) -0.05329(5) -0.33255(10) 0.02818(19) Uani 1 1 d . . .
Cl2 Cl -0.14711(8) -0.27241(5) -0.31753(8) 0.02166(15) Uani 1 1 d . . .
Cl3 Cl -0.30348(9) -0.14106(5) -0.13093(7) 0.02160(15) Uani 1 1 d . . .
Cl4 Cl -0.43725(9) -0.13409(6) -0.44857(7) 0.02254(16) Uani 1 1 d . . .
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
Co 0.01145(16) 0.01387(16) 0.01020(15) 0.00053(13) 0.00208(12) 0.00256(13)
N1 0.0111(10) 0.0224(13) 0.0139(11) -0.0041(9) 0.0024(8) 0.0014(9)
N2 0.0207(13) 0.0166(12) 0.0185(12) 0.0049(10) 0.0056(10) 0.0050(10)
N3 0.0128(11) 0.0139(10) 0.0161(11) 0.0011(9) 0.0014(9) 0.0017(9)
N4 0.0176(12) 0.0150(11) 0.0189(12) 0.0012(9) 0.0049(10) 0.0046(9)
N5 0.0136(11) 0.0154(11) 0.0122(10) 0.0000(8) 0.0004(8) -0.0006(8)
O1 0.0203(11) 0.0193(10) 0.0119(9) -0.0004(8) 0.0004(8) 0.0074(8)
O2 0.0195(12) 0.0331(14) 0.0202(12) -0.0011(10) -0.0081(9) 0.0005(10)
N13 0.0287(16) 0.0229(14) 0.0275(16) -0.0041(12) -0.0035(13) 0.0051(12)
O3 0.0342(16) 0.0289(15) 0.0383(17) 0.0061(12) 0.0064(13) 0.0043(12)
O4 0.043(2) 0.0279(16) 0.051(2) 0.0030(14) -0.0106(16) 0.0128(14)
C10 0.0180(14) 0.0260(16) 0.0126(12) 0.0024(11) 0.0041(10) 0.0003(11)
C11 0.0138(12) 0.0223(14) 0.0153(13) 0.0011(10) 0.0006(10) 0.0062(10)
C12 0.0189(14) 0.0168(13) 0.0141(12) 0.0007(10) -0.0004(10) 0.0016(11)
C13 0.0151(14) 0.0231(16) 0.038(2) -0.0053(14) -0.0011(13) 0.0049(12)
C21 0.0181(13) 0.0173(13) 0.0216(14) 0.0036(11) 0.0041(11) 0.0018(11)
C31 0.0166(13) 0.0155(13) 0.0207(14) 0.0006(11) 0.0018(11) 0.0002(10)
C41 0.0200(15) 0.0182(14) 0.0290(17) -0.0001(12) 0.0068(12) 0.0024(12)
C51 0.0235(16) 0.0195(15) 0.0327(19) -0.0060(13) 0.0104(14) -0.0025(12)
Zn1 0.01325(15) 0.01397(14) 0.01938(16) 0.00117(13) 0.00405(12) 0.00034(13)
Cl1 0.0217(4) 0.0159(3) 0.0474(5) 0.0010(3) 0.0093(4) -0.0017(3)
Cl2 0.0163(3) 0.0157(3) 0.0353(4) 0.0021(3) 0.0108(3) 0.0014(2)
Cl3 0.0228(4) 0.0277(4) 0.0125(3) -0.0007(3) 0.0007(3) -0.0008(3)
Cl4 0.0179(3) 0.0338(4) 0.0154(3) 0.0018(3) 0.0028(3) 0.0060(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
Co O1 1.884(3) . y
Co N1 1.983(3) . y
Co N2 1.976(3) . y
Co N3 1.964(3) . y
Co N4 1.954(3) . y
Co N5 1.959(3) . y
N1 C11 1.452(4) . ?
N1 C10 1.482(4) . ?
N1 H1 0.9601 . ?
N2 C21 1.485(5) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
N3 C31 1.497(4) . ?
N3 H3A 0.9200 . ?
N3 H3B 0.9200 . ?
N4 C41 1.484(5) . ?
N4 H4A 0.9200 . ?
N4 H4B 0.9200 . ?
N5 C51 1.477(5) . ?
N5 H5A 0.9200 . ?
N5 H5B 0.9200 . ?
O1 C12 1.274(4) . ?
O2 C12 1.234(4) . ?
N13 O3 1.222(5) . ?
N13 O4 1.224(5) . ?
N13 C13 1.552(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.500(5) . ?
C11 C12 1.520(5) . ?
C11 H11 1.0000 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C21 C31 1.516(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C41 C51 1.495(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
Zn1 Cl1 2.2521(10) . ?
Zn1 Cl3 2.2733(14) . ?
Zn1 Cl2 2.2794(10) . ?
Zn1 Cl4 2.2841(13) . ?
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
O1 Co N4 86.39(12) . . ?
O1 Co N5 89.42(11) . . ?
N4 Co N5 85.58(12) . . ?
O1 Co N3 176.52(13) . . ?
N4 Co N3 91.73(12) . . ?
N5 Co N3 93.37(11) . . ?
O1 Co N2 91.54(12) . . ?
N4 Co N2 90.43(12) . . ?
N5 Co N2 175.83(12) . . ?
N3 Co N2 85.54(12) . . ?
O1 Co N1 85.53(11) . . ?
N4 Co N1 171.77(12) . . ?
N5 Co N1 92.80(12) . . ?
N3 Co N1 96.41(12) . . ?
N2 Co N1 91.32(12) . . ?
C11 N1 C10 113.0(3) . . ?
C11 N1 Co 108.2(2) . . ?
C10 N1 Co 120.0(2) . . ?
C11 N1 H1 109.3 . . ?
C10 N1 H1 101.4 . . ?
Co N1 H1 103.8 . . ?
C21 N2 Co 109.7(2) . . ?
C21 N2 H2A 109.7 . . ?
Co N2 H2A 109.7 . . ?
C21 N2 H2B 109.7 . . ?
Co N2 H2B 109.7 . . ?
H2A N2 H2B 108.2 . . ?
C31 N3 Co 109.8(2) . . ?
C31 N3 H3A 109.7 . . ?
Co N3 H3A 109.7 . . ?
C31 N3 H3B 109.7 . . ?
Co N3 H3B 109.7 . . ?
H3A N3 H3B 108.2 . . ?
C41 N4 Co 109.6(2) . . ?
C41 N4 H4A 109.8 . . ?
Co N4 H4A 109.8 . . ?
C41 N4 H4B 109.8 . . ?
Co N4 H4B 109.8 . . ?
H4A N4 H4B 108.2 . . ?
C51 N5 Co 109.0(2) . . ?
C51 N5 H5A 109.9 . . ?
Co N5 H5A 109.9 . . ?
C51 N5 H5B 109.9 . . ?
Co N5 H5B 109.9 . . ?
H5A N5 H5B 108.3 . . ?
C12 O1 Co 116.7(2) . . ?
O3 N13 O4 123.9(4) . . ?
O3 N13 C13 118.5(3) . . ?
O4 N13 C13 117.6(4) . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C13 118.2(3) . . ?
N1 C11 C12 111.2(3) . . ?
C13 C11 C12 111.8(3) . . ?
N1 C11 H11 104.8 . . ?
C13 C11 H11 104.8 . . ?
C12 C11 H11 104.8 . . ?
O2 C12 O1 124.6(3) . . ?
O2 C12 C11 119.6(3) . . ?
O1 C12 C11 115.7(3) . . ?
C11 C13 N13 108.8(3) . . ?
C11 C13 H13A 109.9 . . ?
N13 C13 H13A 109.9 . . ?
C11 C13 H13B 109.9 . . ?
N13 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
N2 C21 C31 107.3(3) . . ?
N2 C21 H21A 110.2 . . ?
C31 C21 H21A 110.2 . . ?
N2 C21 H21B 110.2 . . ?
C31 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
N3 C31 C21 107.1(3) . . ?
N3 C31 H31A 110.3 . . ?
C21 C31 H31A 110.3 . . ?
N3 C31 H31B 110.3 . . ?
C21 C31 H31B 110.3 . . ?
H31A C31 H31B 108.6 . . ?
N4 C41 C51 107.1(3) . . ?
N4 C41 H41A 110.3 . . ?
C51 C41 H41A 110.3 . . ?
N4 C41 H41B 110.3 . . ?
C51 C41 H41B 110.3 . . ?
H41A C41 H41B 108.6 . . ?
N5 C51 C41 107.3(3) . . ?
N5 C51 H51A 110.3 . . ?
C41 C51 H51A 110.3 . . ?
N5 C51 H51B 110.3 . . ?
C41 C51 H51B 110.3 . . ?
H51A C51 H51B 108.5 . . ?
Cl1 Zn1 Cl3 114.65(4) . . ?
Cl1 Zn1 Cl2 113.38(4) . . ?
Cl3 Zn1 Cl2 108.41(4) . . ?
Cl1 Zn1 Cl4 105.77(4) . . ?
Cl3 Zn1 Cl4 105.16(5) . . ?
Cl2 Zn1 Cl4 109.00(4) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 Cl1 0.96 2.38 3.276(3) 155.9 .
N1 H1 O3 0.96 2.53 3.035(4) 112.9 .
N2 H2A O3 0.92 2.43 3.192(5) 140.6 .
N2 H2A Cl1 0.92 2.99 3.726(3) 138.6 .
N2 H2B Cl4 0.92 2.66 3.442(3) 143.6 2
N2 H2B Cl1 0.92 3.00 3.729(4) 137.2 2
N3 H3A Cl2 0.92 2.58 3.392(3) 147.7 3_455
N3 H3B Cl3 0.92 2.58 3.358(3) 142.8 2_554
N4 H4A Cl2 0.92 2.70 3.464(3) 140.9 3_455
N4 H4B Cl2 0.92 2.77 3.664(4) 164.4 2
N4 H4B Cl4 0.92 2.81 3.265(3) 111.8 2
N5 H5A Cl3 0.92 2.52 3.333(3) 147.7 3
N5 H5B O2 0.92 2.00 2.828(4) 149.1 4_454
N5 H5A Cl4 0.92 3.10 3.530(3) 110.9 3
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 33.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 2.904
_refine_diff_density_min -1.088
_refine_diff_density_rms 0.186
data_kcd521
_database_code_depnum_ccdc_archive 'CCDC 809639'
#TrackingRef 'CCDC_809638-809639.cif'
_database_code_depnum_ccdc_archive 'CCDC 809639'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
rac-\D*-bis(ethane-1,2-diamine)[(S*)-N-methyl-4-oxo-(R*)-
norvalinato-\k^2^N,O^1^]cobalt(III) tetrachloridozincate
;
_chemical_name_common
;
rac-cdelta*-bis(ethane-1,2-diamine)((S*)-N-methyl-4-oxo-(R*)-
norvalinato-kappa$2!N,O$1!)cobalt(iii) tetrachloridozincate
;
_chemical_melting_point ?
_chemical_formula_moiety 'C10 H26 Co N5 O3, Cl4 Zn'
_chemical_formula_sum 'C10 H26 Cl4 Co N5 O3 Zn'
_chemical_formula_weight 530.46
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 9.1773(6)
_cell_length_b 17.0562(15)
_cell_length_c 12.7279(10)
_cell_angle_alpha 90.00
_cell_angle_beta 105.053(6)
_cell_angle_gamma 90.00
_cell_volume 1923.9(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 122(1)
_cell_measurement_reflns_used 70112
_cell_measurement_theta_min 2.04
_cell_measurement_theta_max 40.00
_exptl_crystal_description prism
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.343
_exptl_crystal_size_mid 0.224
_exptl_crystal_size_min 0.175
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.831
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1080
_exptl_absorpt_coefficient_mu 2.684
_exptl_absorpt_correction_type integration
_exptl_absorpt_correction_T_min 0.541
_exptl_absorpt_correction_T_max 0.689
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 122(1)
_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 'Nonius KappaCCD area-detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_reflns_number 116854
_diffrn_reflns_av_R_equivalents 0.0361
_diffrn_reflns_av_sigmaI/netI 0.0139
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -30
_diffrn_reflns_limit_k_max 30
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 2.04
_diffrn_reflns_theta_max 40.00
_reflns_number_total 11915
_reflns_number_gt 10634
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'COLLECT (Nonius, 1999)'
_computing_cell_refinement 'COLLECT (Nonius, 1999)'
_computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics
;
Ortep-3 (Farrugia, 1997) and Mercury (Macrae et. al., 2006)
;
_computing_publication_material SHELXL-97
_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^)+(0.0188P)^2^+0.9854P] 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 11915
_refine_ls_number_parameters 217
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0277
_refine_ls_R_factor_gt 0.0210
_refine_ls_wR_factor_ref 0.0530
_refine_ls_wR_factor_gt 0.0491
_refine_ls_goodness_of_fit_ref 1.120
_refine_ls_restrained_S_all 1.120
_refine_ls_shift/su_max 0.005
_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
Co Co 0.328802(11) 0.925602(6) 0.302986(8) 0.00730(2) Uani 1 1 d . . .
N1 N 0.46021(7) 0.83264(4) 0.30019(5) 0.00910(9) Uani 1 1 d . . .
H1 H 0.4373 0.7962 0.3512 0.011 Uiso 1 1 d R . .
N2 N 0.31406(7) 0.89600(4) 0.44804(5) 0.00994(9) Uani 1 1 d . . .
H2A H 0.4074 0.8809 0.4899 0.012 Uiso 1 1 calc R . .
H2B H 0.2824 0.9383 0.4811 0.012 Uiso 1 1 calc R . .
N3 N 0.13935(8) 0.86752(4) 0.24944(5) 0.01090(9) Uani 1 1 d . . .
H3A H 0.0717 0.8974 0.1993 0.013 Uiso 1 1 calc R . .
H3B H 0.1571 0.8221 0.2158 0.013 Uiso 1 1 calc R . .
N4 N 0.21855(8) 1.02345(4) 0.30919(5) 0.01097(10) Uani 1 1 d . . .
H4A H 0.1167 1.0135 0.2947 0.013 Uiso 1 1 calc R . .
H4B H 0.2499 1.0452 0.3775 0.013 Uiso 1 1 calc R . .
N5 N 0.33651(8) 0.96159(4) 0.15678(5) 0.01145(10) Uani 1 1 d . . .
H5A H 0.4339 0.9751 0.1576 0.014 Uiso 1 1 calc R . .
H5B H 0.3060 0.9218 0.1071 0.014 Uiso 1 1 calc R . .
O1 O 0.50947(6) 0.98040(3) 0.36825(5) 0.01038(8) Uani 1 1 d . . .
O2 O 0.75212(7) 0.96133(4) 0.45299(5) 0.01244(9) Uani 1 1 d . . .
O3 O 0.60373(7) 0.82559(4) 0.55152(5) 0.01395(10) Uani 1 1 d . . .
C10 C 0.43767(10) 0.78649(5) 0.19760(7) 0.01399(12) Uani 1 1 d . . .
H10A H 0.5101 0.7431 0.2091 0.017 Uiso 1 1 calc R . .
H10B H 0.4533 0.8206 0.1395 0.017 Uiso 1 1 calc R . .
H10C H 0.3348 0.7655 0.1769 0.017 Uiso 1 1 calc R . .
C11 C 0.62140(8) 0.85833(4) 0.33934(6) 0.00954(10) Uani 1 1 d . . .
H11 H 0.6595 0.8651 0.2731 0.011 Uiso 1 1 calc R . .
C12 C 0.63109(8) 0.93866(4) 0.39347(6) 0.00938(10) Uani 1 1 d . . .
C13 C 0.72276(9) 0.79735(5) 0.41009(6) 0.01180(11) Uani 1 1 d . . .
H13A H 0.7115 0.7471 0.3698 0.014 Uiso 1 1 calc R . .
H13B H 0.8290 0.8143 0.4224 0.014 Uiso 1 1 calc R . .
C14 C 0.69073(8) 0.78331(4) 0.51922(6) 0.01047(10) Uani 1 1 d . . .
C15 C 0.77044(9) 0.71610(5) 0.58521(7) 0.01407(12) Uani 1 1 d . . .
H15A H 0.8345 0.6897 0.5454 0.017 Uiso 1 1 calc R . .
H15B H 0.6960 0.6789 0.5988 0.017 Uiso 1 1 calc R . .
H15C H 0.8331 0.7356 0.6547 0.017 Uiso 1 1 calc R . .
C21 C 0.20565(9) 0.83058(5) 0.44005(6) 0.01229(11) Uani 1 1 d . . .
H21A H 0.1704 0.8271 0.5071 0.015 Uiso 1 1 calc R . .
H21B H 0.2536 0.7802 0.4296 0.015 Uiso 1 1 calc R . .
C31 C 0.07518(9) 0.84827(5) 0.34305(7) 0.01307(12) Uani 1 1 d . . .
H31A H 0.0076 0.8022 0.3253 0.016 Uiso 1 1 calc R . .
H31B H 0.0162 0.8932 0.3592 0.016 Uiso 1 1 calc R . .
C41 C 0.24909(10) 1.07850(5) 0.22668(6) 0.01278(11) Uani 1 1 d . . .
H41A H 0.3517 1.1010 0.2522 0.015 Uiso 1 1 calc R . .
H41B H 0.1749 1.1219 0.2129 0.015 Uiso 1 1 calc R . .
C51 C 0.23536(10) 1.03084(5) 0.12472(6) 0.01295(12) Uani 1 1 d . . .
H51A H 0.1297 1.0137 0.0944 0.016 Uiso 1 1 calc R . .
H51B H 0.2668 1.0623 0.0690 0.016 Uiso 1 1 calc R . .
Zn Zn 0.197551(10) 0.891801(5) -0.154955(7) 0.00993(2) Uani 1 1 d . . .
Cl1 Cl 0.08863(2) 0.854730(11) -0.019873(15) 0.01274(3) Uani 1 1 d . . .
Cl2 Cl 0.44406(2) 0.856350(14) -0.099870(19) 0.01853(4) Uani 1 1 d . . .
Cl3 Cl 0.07704(2) 0.828580(13) -0.308798(16) 0.01550(3) Uani 1 1 d . . .
Cl4 Cl 0.17333(3) 1.023221(12) -0.177294(18) 0.01701(4) Uani 1 1 d . . .
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
Co 0.00827(4) 0.00719(4) 0.00661(3) -0.00022(3) 0.00223(3) -0.00047(3)
N1 0.0102(2) 0.0086(2) 0.0092(2) -0.00139(17) 0.00359(17) -0.00099(17)
N2 0.0115(2) 0.0099(2) 0.0087(2) 0.00002(17) 0.00306(18) 0.00026(18)
N3 0.0112(2) 0.0123(2) 0.0094(2) -0.00065(18) 0.00309(18) -0.00166(19)
N4 0.0124(2) 0.0104(2) 0.0101(2) 0.00080(18) 0.00284(19) 0.00127(19)
N5 0.0133(2) 0.0121(2) 0.0093(2) 0.00026(18) 0.00348(19) -0.00072(19)
O1 0.0100(2) 0.00887(19) 0.0118(2) -0.00107(16) 0.00200(16) -0.00017(16)
O2 0.0106(2) 0.0133(2) 0.0125(2) -0.00243(18) 0.00136(17) -0.00165(17)
O3 0.0148(2) 0.0145(2) 0.0141(2) 0.00159(19) 0.00644(19) 0.00446(19)
C10 0.0155(3) 0.0139(3) 0.0128(3) -0.0058(2) 0.0040(2) -0.0004(2)
C11 0.0099(2) 0.0095(2) 0.0101(2) -0.00098(19) 0.0040(2) -0.00083(19)
C12 0.0103(2) 0.0092(2) 0.0092(2) -0.00043(19) 0.00359(19) -0.00105(19)
C13 0.0113(3) 0.0117(3) 0.0135(3) 0.0000(2) 0.0052(2) 0.0019(2)
C14 0.0092(2) 0.0098(2) 0.0122(3) 0.0002(2) 0.0026(2) -0.0001(2)
C15 0.0120(3) 0.0130(3) 0.0162(3) 0.0028(2) 0.0017(2) 0.0021(2)
C21 0.0151(3) 0.0110(3) 0.0123(3) 0.0013(2) 0.0064(2) -0.0013(2)
C31 0.0119(3) 0.0154(3) 0.0133(3) -0.0003(2) 0.0058(2) -0.0027(2)
C41 0.0163(3) 0.0095(3) 0.0123(3) 0.0012(2) 0.0032(2) -0.0004(2)
C51 0.0167(3) 0.0118(3) 0.0095(2) 0.0024(2) 0.0020(2) 0.0000(2)
Zn 0.01027(3) 0.00941(3) 0.00986(3) 0.00006(3) 0.00215(3) 0.00061(3)
Cl1 0.01467(7) 0.01349(7) 0.01082(6) 0.00035(5) 0.00470(5) -0.00022(5)
Cl2 0.01031(7) 0.02129(9) 0.02275(9) 0.00177(7) 0.00209(6) 0.00250(6)
Cl3 0.01745(8) 0.01709(8) 0.01153(7) -0.00363(6) 0.00298(6) -0.00214(6)
Cl4 0.02311(9) 0.00958(7) 0.01873(8) 0.00174(6) 0.00615(7) 0.00099(6)
_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
Co O1 1.8967(6) . y
Co N1 1.9980(7) . y
Co N2 1.9524(7) . y
Co N3 1.9630(7) . y
Co N4 1.9639(7) . y
Co N5 1.9782(7) . y
N1 C10 1.4923(10) . ?
N1 C11 1.4986(10) . ?
N1 H1 0.9599 . ?
N2 C21 1.4808(10) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
N3 C31 1.4962(10) . ?
N3 H3A 0.9200 . ?
N3 H3B 0.9200 . ?
N4 C41 1.4885(10) . ?
N4 H4A 0.9200 . ?
N4 H4B 0.9200 . ?
N5 C51 1.4921(11) . ?
N5 H5A 0.9200 . ?
N5 H5B 0.9200 . ?
O1 C12 1.2920(9) . ?
O2 C12 1.2329(9) . ?
O3 C14 1.2235(10) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.5240(11) . ?
C11 C12 1.5259(10) . ?
C11 H11 1.0000 . ?
C13 C14 1.5117(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.4951(11) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C21 C31 1.5104(12) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C41 C51 1.5086(11) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
Zn Cl3 2.2573(3) . ?
Zn Cl4 2.2631(3) . ?
Zn Cl2 2.2696(3) . ?
Zn Cl1 2.2908(2) . ?
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
O1 Co N2 88.89(3) . . ?
O1 Co N3 174.54(3) . . ?
N2 Co N3 85.71(3) . . ?
O1 Co N4 87.97(3) . . ?
N2 Co N4 91.08(3) . . ?
N3 Co N4 91.36(3) . . ?
O1 Co N5 91.05(3) . . ?
N2 Co N5 176.42(3) . . ?
N3 Co N5 94.29(3) . . ?
N4 Co N5 85.34(3) . . ?
O1 Co N1 86.32(3) . . ?
N2 Co N1 90.11(3) . . ?
N3 Co N1 94.45(3) . . ?
N4 Co N1 174.14(3) . . ?
N5 Co N1 93.46(3) . . ?
C10 N1 C11 110.22(6) . . ?
C10 N1 Co 119.14(5) . . ?
C11 N1 Co 108.08(4) . . ?
C10 N1 H1 104.2 . . ?
C11 N1 H1 109.6 . . ?
Co N1 H1 105.2 . . ?
C21 N2 Co 109.89(5) . . ?
C21 N2 H2A 109.7 . . ?
Co N2 H2A 109.7 . . ?
C21 N2 H2B 109.7 . . ?
Co N2 H2B 109.7 . . ?
H2A N2 H2B 108.2 . . ?
C31 N3 Co 109.30(5) . . ?
C31 N3 H3A 109.8 . . ?
Co N3 H3A 109.8 . . ?
C31 N3 H3B 109.8 . . ?
Co N3 H3B 109.8 . . ?
H3A N3 H3B 108.3 . . ?
C41 N4 Co 108.32(5) . . ?
C41 N4 H4A 110.0 . . ?
Co N4 H4A 110.0 . . ?
C41 N4 H4B 110.0 . . ?
Co N4 H4B 110.0 . . ?
H4A N4 H4B 108.4 . . ?
C51 N5 Co 109.34(5) . . ?
C51 N5 H5A 109.8 . . ?
Co N5 H5A 109.8 . . ?
C51 N5 H5B 109.8 . . ?
Co N5 H5B 109.8 . . ?
H5A N5 H5B 108.3 . . ?
C12 O1 Co 115.96(5) . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C13 113.28(6) . . ?
N1 C11 C12 110.45(6) . . ?
C13 C11 C12 113.01(6) . . ?
N1 C11 H11 106.5 . . ?
C13 C11 H11 106.5 . . ?
C12 C11 H11 106.5 . . ?
O2 C12 O1 124.20(7) . . ?
O2 C12 C11 119.77(7) . . ?
O1 C12 C11 115.93(6) . . ?
C14 C13 C11 114.61(6) . . ?
C14 C13 H13A 108.6 . . ?
C11 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
C11 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
O3 C14 C15 122.00(7) . . ?
O3 C14 C13 121.00(7) . . ?
C15 C14 C13 117.00(7) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C21 C31 106.34(6) . . ?
N2 C21 H21A 110.5 . . ?
C31 C21 H21A 110.5 . . ?
N2 C21 H21B 110.5 . . ?
C31 C21 H21B 110.5 . . ?
H21A C21 H21B 108.7 . . ?
N3 C31 C21 107.60(6) . . ?
N3 C31 H31A 110.2 . . ?
C21 C31 H31A 110.2 . . ?
N3 C31 H31B 110.2 . . ?
C21 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
N4 C41 C51 106.14(6) . . ?
N4 C41 H41A 110.5 . . ?
C51 C41 H41A 110.5 . . ?
N4 C41 H41B 110.5 . . ?
C51 C41 H41B 110.5 . . ?
H41A C41 H41B 108.7 . . ?
N5 C51 C41 106.52(6) . . ?
N5 C51 H51A 110.4 . . ?
C41 C51 H51A 110.4 . . ?
N5 C51 H51B 110.4 . . ?
C41 C51 H51B 110.4 . . ?
H51A C51 H51B 108.6 . . ?
Cl3 Zn Cl4 110.741(10) . . ?
Cl3 Zn Cl2 111.421(11) . . ?
Cl4 Zn Cl2 111.110(9) . . ?
Cl3 Zn Cl1 107.951(9) . . ?
Cl4 Zn Cl1 108.657(9) . . ?
Cl2 Zn Cl1 106.789(10) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O3 0.96 2.66 3.1295(9) 110.8 .
N1 H1 Cl2 0.96 2.67 3.4826(7) 142.3 4_576
N2 H2A O3 0.92 2.00 2.9026(9) 164.9 .
N2 H2B O2 0.92 1.97 2.8766(9) 169.4 3_676
N3 H3A Cl4 0.92 2.58 3.3439(8) 141.2 3_575
N3 H3B Cl3 0.92 2.67 3.4415(8) 142.1 4_576
N4 H4A Cl4 0.92 2.77 3.6400(8) 159.2 3_575
N4 H4B O2 0.92 2.17 2.9798(9) 147.1 3_676
N4 H4B O3 0.92 2.62 3.3061(10) 132.2 3_676
N5 H5B Cl1 0.92 2.50 3.3008(7) 146.4 .
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 40.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.716
_refine_diff_density_min -1.224
_refine_diff_density_rms 0.080