Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2007
data_global
_journal_name_full CrystEngComm
_journal_coden_Cambridge 1350
_publ_contact_author_name 'Larry Falvello'
_publ_contact_author_address
;
Department of Inorganic Chemistry - I.C.M.A.
University of Zaragoza
Calle Pedro Cerbuna, s/n
Zaragoza
E-50009
SPAIN
;
_publ_contact_author_email FALVELLO@UNIZAR.ES
_publ_section_title
;
Using the crystal to engineer the molecule:
Cis-/trans-isomer selection in anionic bis(orotate) complexes
;
_publ_section_references
;
Bruker (2000). SHELXTL-NT. Version 6.10. Bruker AXS Inc., Madison,
Wisconsin, USA.
Bruker (2001a). SMART. Version 5.624. Bruker AXS Inc., Madison,
Wisconsin, USA.
Bruker (2001b). SAINT (Version 6.02a) and SMART (Version
5.625). Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2001c). SADABS. Version 2.03. Bruker AXS Inc., Madison,
Wisconsin, USA.
Oxford (2005a). CrysAlis CCD, Oxford Diffraction Ltd., Version
1.171.26pre9 beta (release 04-02-2005 CrysAlis171 .NET) (compiled Feb 4
2005,10:44:33)
Oxford (2005b). CrysAlis RED, Oxford Diffraction Ltd., Version
1.171.26pre9 beta (release 04-02-2005 CrysAlis171 .NET) (compiled Feb 4
2005,10:44:33)
Sheldrick, G. M. (1990). Acta Cryst. A46, 467--473.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
Siemens (1996). SHELXTL. Version 5.05. Siemens Analytical X-ray
Instruments Inc., Madison, Wisconsin, USA.
;
_publ_contact_author_fax '34 () 976761187'
_publ_contact_author_phone '34 () 976761179'
loop_
_publ_author_name
'Larry Falvello'
'Daniel Ferrer'
'Maria Piedrafita'
'Tatiana Soler'
'Milagros Tomas'
data_1
_database_code_depnum_ccdc_archive 'CCDC 649149'
# exo lrf2L _LRF
#
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C10 H12 N4 Ni O12 2-, 2(Cs +), 2(H2 O)'
_chemical_formula_sum 'C10 H16 Cs2 N4 Ni O14'
_chemical_formula_weight 740.80
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'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.1982(5)
_cell_length_b 8.6340(6)
_cell_length_c 9.2042(7)
_cell_angle_alpha 105.813(1)
_cell_angle_beta 99.892(1)
_cell_angle_gamma 112.181(1)
_cell_volume 484.83(6)
_cell_formula_units_Z 1
_cell_measurement_temperature 100(1)
_cell_measurement_reflns_used 4890
_cell_measurement_theta_min 2.4
_cell_measurement_theta_max 28.7
_exptl_crystal_description plate
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.07
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.537
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 354
_exptl_absorpt_coefficient_mu 4.783
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5836
_exptl_absorpt_correction_T_max 0.7156
_exptl_absorpt_process_details 'Bruker SADABS V2.03'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(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 'CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 85.3
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% .
_diffrn_reflns_number 6020
_diffrn_reflns_av_R_equivalents 0.0156
_diffrn_reflns_av_sigmaI/netI 0.0188
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 2.42
_diffrn_reflns_theta_max 28.82
_reflns_number_total 2299
_reflns_number_gt 2243
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Bruker SMART V5.624'
_computing_cell_refinement 'Bruker SMART V5.624'
_computing_data_reduction 'Bruker SAINT V6.02A'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'SHELXTL Rel. 5.05/V (Siemens, 1996)'
_computing_publication_material 'SHELX-97 (Sheldrick, 1997)'
_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^)+(0.0214P)^2^+0.2052P] 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 mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2299
_refine_ls_number_parameters 174
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0147
_refine_ls_R_factor_gt 0.0140
_refine_ls_wR_factor_ref 0.0363
_refine_ls_wR_factor_gt 0.0359
_refine_ls_goodness_of_fit_ref 1.008
_refine_ls_restrained_S_all 1.008
_refine_ls_shift/su_max 0.001
_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
Ni1 Ni 0.5000 0.5000 0.5000 0.00810(7) Uani 1 2 d S . .
N1 N 0.6174(2) 0.7696(2) 0.52170(17) 0.0092(3) Uani 1 1 d . . .
C2 C 0.7729(3) 0.9200(2) 0.6408(2) 0.0088(3) Uani 1 1 d . . .
O2 O 0.8411(2) 0.92601(17) 0.77656(14) 0.0123(3) Uani 1 1 d . . .
N3 N 0.8600(2) 1.0753(2) 0.60840(17) 0.0097(3) Uani 1 1 d . . .
H3 H 0.960(4) 1.170(4) 0.686(3) 0.029(7) Uiso 1 1 d . . .
C4 C 0.7889(3) 1.0953(2) 0.4700(2) 0.0090(3) Uani 1 1 d . . .
O4 O 0.8773(2) 1.24328(17) 0.45385(15) 0.0123(3) Uani 1 1 d . . .
C5 C 0.6147(3) 0.9399(2) 0.3526(2) 0.0103(3) Uani 1 1 d . . .
H5 H 0.560(4) 0.941(3) 0.254(3) 0.011(5) Uiso 1 1 d . . .
C6 C 0.5412(3) 0.7862(2) 0.3841(2) 0.0091(3) Uani 1 1 d . . .
C7 C 0.3615(3) 0.6137(2) 0.2593(2) 0.0095(3) Uani 1 1 d . . .
O5 O 0.3253(2) 0.47131(17) 0.28809(14) 0.0118(2) Uani 1 1 d . . .
O6 O 0.2627(2) 0.62131(17) 0.13868(15) 0.0128(3) Uani 1 1 d . . .
Cs1 Cs 1.131376(16) 0.787306(14) 0.913579(12) 0.01166(4) Uani 1 1 d . . .
O1W O 0.7342(2) 0.48006(19) 0.39733(15) 0.0111(2) Uani 1 1 d . . .
H1A H 0.853(4) 0.573(4) 0.443(3) 0.027(7) Uiso 1 1 d . . .
H1B H 0.753(4) 0.395(4) 0.405(3) 0.030(7) Uiso 1 1 d . . .
O2W O 0.7711(2) 0.62074(18) 0.14142(17) 0.0149(3) Uani 1 1 d . . .
H2A H 0.723(4) 0.554(4) 0.183(3) 0.025(7) Uiso 1 1 d . . .
H2B H 0.770(5) 0.551(5) 0.050(4) 0.056(10) Uiso 1 1 d . . .
O3W O 1.4201(2) 1.2065(2) 1.03873(18) 0.0167(3) Uani 1 1 d . . .
H3A H 1.374(5) 1.223(4) 1.111(4) 0.043(9) Uiso 1 1 d . . .
H3B H 1.377(4) 1.254(4) 0.980(3) 0.028(7) Uiso 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
Ni1 0.00829(15) 0.00710(15) 0.00789(14) 0.00314(12) 0.00122(11) 0.00272(12)
N1 0.0096(7) 0.0094(7) 0.0091(6) 0.0034(5) 0.0026(6) 0.0047(6)
C2 0.0089(8) 0.0095(8) 0.0103(7) 0.0042(6) 0.0044(6) 0.0053(6)
O2 0.0133(6) 0.0117(6) 0.0103(6) 0.0042(5) 0.0015(5) 0.0047(5)
N3 0.0104(7) 0.0078(7) 0.0089(7) 0.0025(6) 0.0017(6) 0.0029(6)
C4 0.0099(8) 0.0105(8) 0.0102(7) 0.0046(6) 0.0051(6) 0.0067(7)
O4 0.0113(6) 0.0102(6) 0.0143(6) 0.0061(5) 0.0026(5) 0.0032(5)
C5 0.0108(8) 0.0106(8) 0.0109(8) 0.0048(6) 0.0040(7) 0.0053(7)
C6 0.0079(8) 0.0109(8) 0.0100(7) 0.0032(6) 0.0038(6) 0.0056(7)
C7 0.0102(8) 0.0094(8) 0.0100(7) 0.0031(6) 0.0051(6) 0.0052(7)
O5 0.0121(6) 0.0082(6) 0.0121(6) 0.0039(5) 0.0005(5) 0.0030(5)
O6 0.0140(6) 0.0127(6) 0.0096(6) 0.0048(5) 0.0004(5) 0.0049(5)
Cs1 0.01041(6) 0.01180(7) 0.01189(6) 0.00509(5) 0.00130(4) 0.00453(5)
O1W 0.0103(6) 0.0085(6) 0.0129(6) 0.0041(5) 0.0020(5) 0.0031(5)
O2W 0.0167(7) 0.0111(6) 0.0138(6) 0.0036(5) 0.0039(5) 0.0042(5)
O3W 0.0183(7) 0.0188(7) 0.0170(7) 0.0083(6) 0.0092(6) 0.0095(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
Ni1 O5 2.0264(12) . ?
Ni1 N1 2.0922(15) . ?
Ni1 O1W 2.1077(13) . ?
N1 C2 1.358(2) . ?
N1 C6 1.359(2) . ?
C2 O2 1.241(2) . ?
C2 N3 1.388(2) . ?
O2 Cs1 3.0329(13) . ?
N3 C4 1.370(2) . ?
N3 H3 0.87(3) . ?
C4 O4 1.258(2) . ?
C4 C5 1.419(2) . ?
C5 C6 1.362(2) . ?
C5 H5 0.93(2) . ?
C6 C7 1.521(2) . ?
C7 O6 1.243(2) . ?
C7 O5 1.269(2) . ?
Cs1 O6 3.0347(13) 1_656 ?
Cs1 O5 3.0560(13) 2_666 ?
Cs1 O2 3.1445(13) 2_777 ?
Cs1 O3W 3.1580(15) . ?
Cs1 O3W 3.1605(15) 2_877 ?
Cs1 O4 3.3073(13) 2_776 ?
Cs1 O6 3.4315(13) 2_666 ?
Cs1 C7 3.5904(18) 2_666 ?
O1W H1A 0.85(3) . ?
O1W H1B 0.81(3) . ?
O2W H2A 0.79(3) . ?
O2W H2B 0.89(4) . ?
O3W H3A 0.79(3) . ?
O3W H3B 0.84(3) . ?
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
O5 Ni1 N1 99.95(5) . 2_666 ?
O5 Ni1 N1 80.05(5) . . ?
O5 Ni1 O1W 90.63(5) . 2_666 ?
N1 Ni1 O1W 91.25(5) . 2_666 ?
O5 Ni1 O1W 89.37(5) . . ?
N1 Ni1 O1W 88.75(5) . . ?
C2 N1 C6 117.62(15) . . ?
C2 N1 Ni1 129.97(12) . . ?
C6 N1 Ni1 111.72(11) . . ?
O2 C2 N1 123.62(16) . . ?
O2 C2 N3 118.34(16) . . ?
N1 C2 N3 118.04(15) . . ?
C2 O2 Cs1 132.77(11) . . ?
C2 O2 Cs1 123.62(11) . 2_777 ?
Cs1 O2 Cs1 100.90(4) . 2_777 ?
C4 N3 C2 125.30(15) . . ?
C4 N3 H3 118.0(18) . . ?
C2 N3 H3 116.4(18) . . ?
O4 C4 N3 120.21(16) . . ?
O4 C4 C5 124.68(16) . . ?
N3 C4 C5 115.11(15) . . ?
C4 O4 Cs1 114.96(10) . 2_776 ?
C6 C5 C4 118.19(16) . . ?
C6 C5 H5 121.0(14) . . ?
C4 C5 H5 120.6(14) . . ?
N1 C6 C5 125.31(16) . . ?
N1 C6 C7 114.39(15) . . ?
C5 C6 C7 120.30(15) . . ?
O6 C7 O5 125.09(17) . . ?
O6 C7 C6 118.83(16) . . ?
O5 C7 C6 116.07(15) . . ?
C7 O5 Ni1 116.77(11) . . ?
C7 O5 Cs1 104.51(10) . 2_666 ?
Ni1 O5 Cs1 131.77(5) . 2_666 ?
C7 O6 Cs1 158.54(12) . 1_454 ?
C7 O6 Cs1 87.11(10) . 2_666 ?
Cs1 O6 Cs1 112.55(4) 1_454 2_666 ?
O2 Cs1 O6 151.43(4) . 1_656 ?
O2 Cs1 O5 59.38(3) . 2_666 ?
O6 Cs1 O5 107.11(3) 1_656 2_666 ?
O2 Cs1 O2 79.10(4) . 2_777 ?
O6 Cs1 O2 84.25(3) 1_656 2_777 ?
O5 Cs1 O2 111.82(3) 2_666 2_777 ?
O2 Cs1 O3W 76.80(4) . . ?
O6 Cs1 O3W 111.57(4) 1_656 . ?
O5 Cs1 O3W 136.18(4) 2_666 . ?
O2 Cs1 O3W 54.29(4) 2_777 . ?
O2 Cs1 O3W 145.73(4) . 2_877 ?
O6 Cs1 O3W 61.78(4) 1_656 2_877 ?
O5 Cs1 O3W 138.08(4) 2_666 2_877 ?
O2 Cs1 O3W 107.16(4) 2_777 2_877 ?
O3W Cs1 O3W 80.14(4) . 2_877 ?
O2 Cs1 O4 68.45(3) . 2_776 ?
O6 Cs1 O4 136.06(3) 1_656 2_776 ?
O5 Cs1 O4 75.26(3) 2_666 2_776 ?
O2 Cs1 O4 136.96(3) 2_777 2_776 ?
O3W Cs1 O4 90.28(4) . 2_776 ?
O3W Cs1 O4 86.80(4) 2_877 2_776 ?
O2 Cs1 O6 95.70(3) . 2_666 ?
O6 Cs1 O6 67.45(4) 1_656 2_666 ?
O5 Cs1 O6 39.66(3) 2_666 2_666 ?
O2 Cs1 O6 107.69(3) 2_777 2_666 ?
O3W Cs1 O6 161.23(3) . 2_666 ?
O3W Cs1 O6 113.30(4) 2_877 2_666 ?
O4 Cs1 O6 103.08(3) 2_776 2_666 ?
Ni1 O1W Cs1 147.40(6) . 2_766 ?
Ni1 O1W H1A 113.0(17) . . ?
Cs1 O1W H1A 99.6(17) 2_766 . ?
Ni1 O1W H1B 109.9(19) . . ?
Cs1 O1W H1B 58.8(19) 2_766 . ?
H1A O1W H1B 107(3) . . ?
Cs1 O2W Cs1 91.86(3) 1_554 2_766 ?
Cs1 O2W H2A 151(2) 1_554 . ?
Cs1 O2W H2A 59.5(19) 2_766 . ?
Cs1 O2W H2B 57(2) 1_554 . ?
Cs1 O2W H2B 55(2) 2_766 . ?
H2A O2W H2B 104(3) . . ?
Cs1 O3W Cs1 99.86(4) . 2_877 ?
Cs1 O3W H3A 91(2) . . ?
Cs1 O3W H3A 121(2) 2_877 . ?
Cs1 O3W H3B 111.6(19) . . ?
Cs1 O3W H3B 122.2(19) 2_877 . ?
H3A O3W H3B 106(3) . . ?
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
N3 H3 O2W 0.87(3) 2.06(3) 2.930(2) 171(3) 2_776
O1W H1A O4 0.85(3) 1.85(3) 2.6942(19) 174(3) 2_776
O1W H1B O4 0.81(3) 1.95(3) 2.7383(18) 164(3) 1_545
O2W H2A O1W 0.79(3) 2.23(3) 2.937(2) 150(3) .
O2W H2B O6 0.89(4) 1.86(4) 2.7452(18) 172(3) 2_665
O3W H3A O2 0.79(3) 2.21(3) 2.876(2) 141(3) 2_777
O3W H3A O5 0.79(3) 2.50(3) 3.1332(19) 138(3) 1_666
O3W H3B O2W 0.84(3) 2.17(3) 2.997(2) 169(3) 2_776
_diffrn_measured_fraction_theta_max 0.904
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.433
_refine_diff_density_min -0.459
_refine_diff_density_rms 0.095
# Formatted by publCIF
#===END
data_2
_database_code_depnum_ccdc_archive 'CCDC 649150'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C16 H36 N), C10 H8 N4 Ni O10, 2(H2 O)'
_chemical_formula_sum 'C42 H84 N6 Ni O12'
_chemical_formula_weight 923.86
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.1915(4)
_cell_length_b 12.3098(6)
_cell_length_c 16.4178(7)
_cell_angle_alpha 90.374(4)
_cell_angle_beta 96.009(3)
_cell_angle_gamma 95.849(3)
_cell_volume 2437.24(18)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(1)
_cell_measurement_reflns_used 7540
_cell_measurement_theta_min 3.20
_cell_measurement_theta_max 27.33
_exptl_crystal_description plate
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.259
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1004
_exptl_absorpt_coefficient_mu 0.461
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.711
_exptl_absorpt_correction_T_max 0.977
_exptl_absorpt_process_details 'Bruker SADABS V2.03'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(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 'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method '\w and \f scans'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% .
_diffrn_reflns_number 19690
_diffrn_reflns_av_R_equivalents 0.0547
_diffrn_reflns_av_sigmaI/netI 0.0784
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 3.89
_diffrn_reflns_theta_max 25.00
_reflns_number_total 8544
_reflns_number_gt 6734
_reflns_threshold_expression I>2\s(I)
_computing_data_collection
;
CrysAlis CCD (Oxford, 2005)
;
_computing_cell_refinement
;
CrysAlis RED (Oxford, 2005)
;
_computing_data_reduction
;
CrysAlis RED (Oxford, 2005)
;
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'SHELXTL (Bruker, 2000)'
_computing_publication_material 'SHELX-97 (Sheldrick, 1997)'
_publ_section_exptl_refinement
;
Hydrogen atoms of the two coordinated water molecules were located in a
difference Fourier map and refined freely. For one of the unligated water
molecules, O3W, the hydrogen atoms were not located and are likely to be
disordered. For the second free water molecule, O4W, the hydrogen atoms were
located in a difference Fourier map; they were refined with similarity
restraints (on the O---H distances) and their isotropic U values were
constrained to 1.2 times the equivalent isotropic U value of O4W. Methyl
hydrogen atoms were located in a local slant Fourier calculation and the
methyl groups were refined as rigid rotators with U(iso)(H) set to 1.2 times
U(eq) of the parent carbon atoms. All other hydrogen atoms were placed in
calculated positions and refined as riding atoms with their U(iso) values
constrained to 1.2 times the U(eq) values of their respective carrier atoms.
Omit maps were made (PLATON) to check the correct location of H1WB and H4A,
for which CheckCIF signals a close contact. Both seem to be correctly placed.
An omit map also shows what might be a minor disorder component for H4B, but
that possibility was not pursued for the structural model. H4A is within
'contact' distance to both O1W and O3W, but the O4W---H4A...O angles in
both cases are too narrow, in our opinion, for either of these contacts
to be called a hydrogen bond.
;
_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^)+(0.0318P)^2^+4.1949P] 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 mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8544
_refine_ls_number_parameters 580
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.1034
_refine_ls_R_factor_gt 0.0758
_refine_ls_wR_factor_ref 0.1422
_refine_ls_wR_factor_gt 0.1316
_refine_ls_goodness_of_fit_ref 1.139
_refine_ls_restrained_S_all 1.139
_refine_ls_shift/su_max 0.003
_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
Ni1 Ni 0.79352(4) 0.06777(4) 0.33110(3) 0.01974(15) Uani 1 1 d . . .
N1 N 0.7087(3) 0.0066(3) 0.22191(19) 0.0201(7) Uani 1 1 d . . .
C2 C 0.6098(3) 0.0300(3) 0.1850(2) 0.0217(9) Uani 1 1 d . . .
O2 O 0.5436(2) 0.0801(2) 0.22164(16) 0.0286(7) Uani 1 1 d . . .
N3 N 0.5806(3) -0.0007(3) 0.10430(18) 0.0195(7) Uani 1 1 d . . .
H3 H 0.5166 0.0169 0.0811 0.023 Uiso 1 1 calc R . .
C4 C 0.6437(3) -0.0569(3) 0.0568(2) 0.0215(9) Uani 1 1 d . . .
O4 O 0.6119(2) -0.0757(2) -0.01800(16) 0.0261(7) Uani 1 1 d . . .
C5 C 0.7424(3) -0.0885(3) 0.0997(2) 0.0194(9) Uani 1 1 d . . .
H5 H 0.7878 -0.1335 0.0738 0.023 Uiso 1 1 calc R . .
C6 C 0.7707(3) -0.0539(3) 0.1775(2) 0.0194(9) Uani 1 1 d . . .
O5 O 0.9075(2) -0.0300(2) 0.29292(15) 0.0226(6) Uani 1 1 d . . .
C7 C 0.8801(3) -0.0806(3) 0.2246(2) 0.0223(9) Uani 1 1 d . . .
O6 O 0.9322(2) -0.1473(3) 0.19297(18) 0.0328(7) Uani 1 1 d . . .
N11 N 0.8965(3) 0.1284(3) 0.43161(18) 0.0212(8) Uani 1 1 d . . .
C12 C 0.9098(3) 0.0898(3) 0.5085(2) 0.0218(9) Uani 1 1 d . . .
O12 O 0.8442(2) 0.0150(2) 0.53385(15) 0.0264(7) Uani 1 1 d . . .
N13 N 0.9993(3) 0.1337(3) 0.56213(19) 0.0244(8) Uani 1 1 d . . .
H13 H 1.0070 0.1065 0.6116 0.029 Uiso 1 1 calc R . .
C14 C 1.0767(3) 0.2166(3) 0.5436(2) 0.0266(10) Uani 1 1 d . . .
O14 O 1.1576(2) 0.2467(2) 0.59457(17) 0.0332(7) Uani 1 1 d . . .
C15 C 1.0559(3) 0.2598(4) 0.4635(2) 0.0263(10) Uani 1 1 d . . .
H15 H 1.1024 0.3203 0.4464 0.032 Uiso 1 1 calc R . .
C16 C 0.9690(3) 0.2136(3) 0.4119(2) 0.0201(9) Uani 1 1 d . . .
O15 O 0.8678(2) 0.2016(2) 0.27980(15) 0.0246(6) Uani 1 1 d . . .
C17 C 0.9455(3) 0.2564(3) 0.3252(2) 0.0232(9) Uani 1 1 d . . .
O16 O 1.0042(2) 0.3383(2) 0.30492(17) 0.0295(7) Uani 1 1 d . . .
O1W O 0.6658(3) 0.1597(3) 0.3590(2) 0.0294(7) Uani 1 1 d . . .
H1WA H 0.607(5) 0.151(5) 0.314(4) 0.09(2) Uiso 1 1 d . . .
H1WB H 0.644(4) 0.141(4) 0.402(3) 0.036(15) Uiso 1 1 d . . .
O2W O 0.7270(2) -0.0664(3) 0.39805(19) 0.0258(7) Uani 1 1 d . . .
H2WA H 0.758(4) -0.122(5) 0.387(3) 0.050(17) Uiso 1 1 d . . .
H2WB H 0.756(4) -0.044(4) 0.451(3) 0.045(14) Uiso 1 1 d . . .
O3W O 0.4995(3) -0.0683(3) 0.3621(3) 0.0680(12) Uani 1 1 d . . .
O4W O 0.6401(4) 0.1165(5) 0.5210(3) 0.0803(15) Uani 1 1 d D . .
H4A H 0.586(4) 0.058(4) 0.500(4) 0.096 Uiso 1 1 d D . .
H4B H 0.706(3) 0.080(5) 0.529(4) 0.096 Uiso 1 1 d D . .
N21 N 0.2306(3) 0.1443(3) 0.22875(19) 0.0228(8) Uani 1 1 d . . .
C21 C 0.2489(3) 0.1771(4) 0.3194(2) 0.0248(9) Uani 1 1 d . . .
H21A H 0.2281 0.2523 0.3252 0.030 Uiso 1 1 calc R . .
H21B H 0.1979 0.1282 0.3492 0.030 Uiso 1 1 calc R . .
C22 C 0.3657(3) 0.1737(4) 0.3604(2) 0.0322(11) Uani 1 1 d . . .
H22A H 0.4195 0.2070 0.3243 0.039 Uiso 1 1 calc R . .
H22B H 0.3804 0.0969 0.3694 0.039 Uiso 1 1 calc R . .
C23 C 0.3814(4) 0.2356(4) 0.4426(3) 0.0347(11) Uani 1 1 d . . .
H23A H 0.3169 0.2140 0.4731 0.042 Uiso 1 1 calc R . .
H23B H 0.4483 0.2139 0.4752 0.042 Uiso 1 1 calc R . .
C24 C 0.3931(6) 0.3575(5) 0.4341(4) 0.0705(19) Uani 1 1 d . . .
H24A H 0.4574 0.3798 0.4046 0.085 Uiso 1 1 calc R . .
H24B H 0.4037 0.3923 0.4886 0.085 Uiso 1 1 calc R . .
H24C H 0.3260 0.3801 0.4036 0.085 Uiso 1 1 calc R . .
C25 C 0.2585(3) 0.0289(3) 0.2152(2) 0.0227(9) Uani 1 1 d . . .
H25A H 0.2420 0.0103 0.1561 0.027 Uiso 1 1 calc R . .
H25B H 0.3392 0.0272 0.2295 0.027 Uiso 1 1 calc R . .
C26 C 0.1982(3) -0.0583(3) 0.2630(2) 0.0245(9) Uani 1 1 d . . .
H26A H 0.1173 -0.0534 0.2535 0.029 Uiso 1 1 calc R . .
H26B H 0.2215 -0.0467 0.3223 0.029 Uiso 1 1 calc R . .
C27 C 0.2237(4) -0.1712(4) 0.2365(3) 0.0302(10) Uani 1 1 d . . .
H27A H 0.1965 -0.1844 0.1780 0.036 Uiso 1 1 calc R . .
H27B H 0.3049 -0.1746 0.2429 0.036 Uiso 1 1 calc R . .
C28 C 0.1690(4) -0.2588(4) 0.2876(3) 0.0335(11) Uani 1 1 d . . .
H28A H 0.1957 -0.2456 0.3455 0.040 Uiso 1 1 calc R . .
H28B H 0.1874 -0.3306 0.2704 0.040 Uiso 1 1 calc R . .
H28C H 0.0884 -0.2571 0.2798 0.040 Uiso 1 1 calc R . .
C29 C 0.3053(3) 0.2178(3) 0.1793(2) 0.0258(10) Uani 1 1 d . . .
H29A H 0.3833 0.2096 0.1996 0.031 Uiso 1 1 calc R . .
H29B H 0.2934 0.1917 0.1216 0.031 Uiso 1 1 calc R . .
C30 C 0.2893(4) 0.3381(4) 0.1812(3) 0.0358(11) Uani 1 1 d . . .
H30A H 0.3000 0.3657 0.2386 0.043 Uiso 1 1 calc R . .
H30B H 0.2128 0.3486 0.1583 0.043 Uiso 1 1 calc R . .
C31 C 0.3723(4) 0.4021(4) 0.1312(3) 0.0382(12) Uani 1 1 d . . .
H31A H 0.3667 0.4811 0.1387 0.046 Uiso 1 1 calc R . .
H31B H 0.4482 0.3876 0.1529 0.046 Uiso 1 1 calc R . .
C32 C 0.3556(4) 0.3747(4) 0.0414(3) 0.0434(13) Uani 1 1 d . . .
H32A H 0.3660 0.2977 0.0330 0.052 Uiso 1 1 calc R . .
H32B H 0.4096 0.4207 0.0131 0.052 Uiso 1 1 calc R . .
H32C H 0.2804 0.3878 0.0193 0.052 Uiso 1 1 calc R . .
C33 C 0.1080(3) 0.1553(3) 0.2029(2) 0.0227(9) Uani 1 1 d . . .
H33A H 0.0632 0.1096 0.2392 0.027 Uiso 1 1 calc R . .
H33B H 0.0944 0.2321 0.2118 0.027 Uiso 1 1 calc R . .
C34 C 0.0674(3) 0.1228(4) 0.1147(2) 0.0274(10) Uani 1 1 d . . .
H34A H 0.0546 0.0422 0.1094 0.033 Uiso 1 1 calc R . .
H34B H 0.1245 0.1488 0.0786 0.033 Uiso 1 1 calc R . .
C35 C -0.0402(3) 0.1725(4) 0.0885(2) 0.0293(10) Uani 1 1 d . . .
H35A H -0.0935 0.1543 0.1291 0.035 Uiso 1 1 calc R . .
H35B H -0.0249 0.2530 0.0876 0.035 Uiso 1 1 calc R . .
C36 C -0.0917(4) 0.1308(4) 0.0044(3) 0.0321(11) Uani 1 1 d . . .
H36A H -0.0383 0.1469 -0.0357 0.039 Uiso 1 1 calc R . .
H36B H -0.1585 0.1670 -0.0114 0.039 Uiso 1 1 calc R . .
H36C H -0.1114 0.0518 0.0061 0.039 Uiso 1 1 calc R . .
N22 N 0.7542(3) 0.5114(3) 0.22224(19) 0.0215(7) Uani 1 1 d . . .
C37 C 0.7322(4) 0.3949(3) 0.1891(2) 0.0245(9) Uani 1 1 d . . .
H37A H 0.6775 0.3544 0.2212 0.029 Uiso 1 1 calc R . .
H37B H 0.8020 0.3599 0.1982 0.029 Uiso 1 1 calc R . .
C38 C 0.6893(3) 0.3832(3) 0.0984(2) 0.0259(10) Uani 1 1 d . . .
H38A H 0.6242 0.4248 0.0872 0.031 Uiso 1 1 calc R . .
H38B H 0.7476 0.4142 0.0650 0.031 Uiso 1 1 calc R . .
C39 C 0.6564(4) 0.2635(4) 0.0741(3) 0.0299(10) Uani 1 1 d . . .
H39A H 0.7205 0.2215 0.0883 0.036 Uiso 1 1 calc R . .
H39B H 0.5957 0.2339 0.1058 0.036 Uiso 1 1 calc R . .
C40 C 0.6185(4) 0.2483(4) -0.0170(3) 0.0337(11) Uani 1 1 d . . .
H40A H 0.5498 0.2824 -0.0302 0.040 Uiso 1 1 calc R . .
H40B H 0.6054 0.1701 -0.0308 0.040 Uiso 1 1 calc R . .
H40C H 0.6761 0.2825 -0.0487 0.040 Uiso 1 1 calc R . .
C41 C 0.6446(3) 0.5589(3) 0.2219(2) 0.0251(9) Uani 1 1 d . . .
H41A H 0.5968 0.5118 0.2554 0.030 Uiso 1 1 calc R . .
H41B H 0.6081 0.5551 0.1651 0.030 Uiso 1 1 calc R . .
C42 C 0.6487(3) 0.6754(4) 0.2532(3) 0.0324(11) Uani 1 1 d . . .
H42A H 0.6897 0.7253 0.2172 0.039 Uiso 1 1 calc R . .
H42B H 0.6883 0.6822 0.3091 0.039 Uiso 1 1 calc R . .
C43 C 0.5308(4) 0.7075(4) 0.2548(3) 0.0383(12) Uani 1 1 d . . .
H43A H 0.5346 0.7877 0.2626 0.046 Uiso 1 1 calc R . .
H43B H 0.4882 0.6885 0.2010 0.046 Uiso 1 1 calc R . .
C44 C 0.4692(5) 0.6525(5) 0.3216(4) 0.0628(17) Uani 1 1 d . . .
H44A H 0.4577 0.5735 0.3109 0.075 Uiso 1 1 calc R . .
H44B H 0.3972 0.6812 0.3222 0.075 Uiso 1 1 calc R . .
H44C H 0.5129 0.6672 0.3748 0.075 Uiso 1 1 calc R . .
C45 C 0.8290(3) 0.5817(3) 0.1709(2) 0.0232(9) Uani 1 1 d . . .
H45A H 0.7868 0.5932 0.1174 0.028 Uiso 1 1 calc R . .
H45B H 0.8473 0.6540 0.1984 0.028 Uiso 1 1 calc R . .
C46 C 0.9361(3) 0.5371(4) 0.1555(3) 0.0282(10) Uani 1 1 d . . .
H46A H 0.9199 0.4653 0.1269 0.034 Uiso 1 1 calc R . .
H46B H 0.9808 0.5269 0.2083 0.034 Uiso 1 1 calc R . .
C47 C 1.0008(3) 0.6169(4) 0.1031(3) 0.0325(11) Uani 1 1 d . . .
H47A H 0.9549 0.6273 0.0509 0.039 Uiso 1 1 calc R . .
H47B H 1.0160 0.6885 0.1320 0.039 Uiso 1 1 calc R . .
C48 C 1.1093(4) 0.5773(4) 0.0849(3) 0.0466(14) Uani 1 1 d . . .
H48A H 1.1583 0.5747 0.1359 0.056 Uiso 1 1 calc R . .
H48B H 1.1448 0.6275 0.0471 0.056 Uiso 1 1 calc R . .
H48C H 1.0951 0.5041 0.0598 0.056 Uiso 1 1 calc R . .
C49 C 0.8128(4) 0.5106(4) 0.3090(2) 0.0282(10) Uani 1 1 d . . .
H49A H 0.8835 0.4783 0.3067 0.034 Uiso 1 1 calc R . .
H49B H 0.8313 0.5872 0.3285 0.034 Uiso 1 1 calc R . .
C50 C 0.7489(4) 0.4491(4) 0.3719(3) 0.0391(12) Uani 1 1 d . . .
H50A H 0.7318 0.3713 0.3553 0.047 Uiso 1 1 calc R . .
H50B H 0.6782 0.4806 0.3765 0.047 Uiso 1 1 calc R . .
C51 C 0.8218(6) 0.4597(4) 0.4541(3) 0.0606(18) Uani 1 1 d . . .
H51A H 0.8938 0.4317 0.4476 0.073 Uiso 1 1 calc R . .
H51B H 0.8366 0.5377 0.4705 0.073 Uiso 1 1 calc R . .
C52 C 0.7672(8) 0.3969(6) 0.5208(3) 0.101(3) Uani 1 1 d . . .
H52A H 0.6936 0.4207 0.5247 0.121 Uiso 1 1 calc R . .
H52B H 0.8129 0.4109 0.5733 0.121 Uiso 1 1 calc R . .
H52C H 0.7599 0.3186 0.5076 0.121 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
Ni1 0.0207(3) 0.0230(3) 0.0148(3) 0.0017(2) -0.0020(2) 0.0029(2)
N1 0.0172(17) 0.0232(19) 0.0195(17) 0.0034(14) 0.0004(14) 0.0019(14)
C2 0.023(2) 0.022(2) 0.019(2) 0.0017(17) -0.0003(17) -0.0022(18)
O2 0.0227(15) 0.0405(19) 0.0236(15) -0.0062(13) 0.0002(12) 0.0102(14)
N3 0.0153(17) 0.025(2) 0.0176(16) 0.0002(14) -0.0029(13) 0.0027(14)
C4 0.022(2) 0.019(2) 0.022(2) 0.0001(17) -0.0004(17) -0.0021(17)
O4 0.0256(15) 0.0337(18) 0.0185(15) -0.0013(12) -0.0027(12) 0.0065(13)
C5 0.017(2) 0.021(2) 0.020(2) 0.0007(17) 0.0017(16) 0.0018(17)
C6 0.016(2) 0.019(2) 0.024(2) 0.0054(17) 0.0026(16) 0.0006(16)
O5 0.0226(15) 0.0263(16) 0.0181(14) 0.0001(12) -0.0039(11) 0.0051(12)
C7 0.024(2) 0.018(2) 0.024(2) 0.0043(18) -0.0002(17) -0.0005(18)
O6 0.0293(17) 0.0358(19) 0.0333(17) -0.0073(14) -0.0052(13) 0.0129(14)
N11 0.0258(18) 0.025(2) 0.0137(16) -0.0003(14) -0.0016(14) 0.0091(15)
C12 0.025(2) 0.024(2) 0.018(2) -0.0037(17) 0.0000(17) 0.0095(19)
O12 0.0325(16) 0.0303(17) 0.0159(14) 0.0021(12) 0.0012(12) 0.0013(14)
N13 0.030(2) 0.026(2) 0.0161(17) -0.0003(15) -0.0060(14) 0.0073(16)
C14 0.031(2) 0.022(2) 0.026(2) -0.0038(18) -0.0034(19) 0.007(2)
O14 0.0369(18) 0.0278(18) 0.0305(16) -0.0031(13) -0.0186(14) 0.0054(14)
C15 0.029(2) 0.025(2) 0.025(2) 0.0023(18) -0.0020(18) 0.0070(19)
C16 0.024(2) 0.019(2) 0.018(2) 0.0001(16) 0.0005(16) 0.0056(17)
O15 0.0289(16) 0.0259(16) 0.0176(14) 0.0034(12) -0.0042(12) 0.0023(13)
C17 0.027(2) 0.025(2) 0.020(2) 0.0003(18) 0.0025(18) 0.0121(19)
O16 0.0367(17) 0.0241(17) 0.0278(16) 0.0056(13) 0.0054(13) 0.0007(14)
O1W 0.0307(18) 0.039(2) 0.0204(17) 0.0029(15) 0.0013(15) 0.0129(15)
O2W 0.0249(16) 0.0289(19) 0.0228(17) 0.0027(14) -0.0005(13) 0.0026(14)
O3W 0.054(2) 0.065(3) 0.086(3) 0.011(2) 0.010(2) 0.005(2)
O4W 0.081(3) 0.120(5) 0.049(3) 0.013(3) 0.008(2) 0.050(3)
N21 0.0196(18) 0.027(2) 0.0214(18) -0.0004(15) 0.0013(14) 0.0022(15)
C21 0.029(2) 0.026(2) 0.019(2) -0.0022(17) 0.0012(17) 0.0025(19)
C22 0.030(2) 0.044(3) 0.022(2) 0.000(2) -0.0030(19) 0.006(2)
C23 0.035(3) 0.041(3) 0.026(2) 0.000(2) -0.004(2) 0.002(2)
C24 0.099(5) 0.045(4) 0.056(4) -0.004(3) -0.033(4) -0.005(3)
C25 0.021(2) 0.022(2) 0.025(2) 0.0012(17) 0.0034(17) 0.0030(18)
C26 0.020(2) 0.032(3) 0.020(2) 0.0049(18) 0.0017(17) -0.0013(18)
C27 0.031(2) 0.028(3) 0.031(2) 0.006(2) 0.0025(19) 0.004(2)
C28 0.045(3) 0.025(3) 0.028(2) 0.0047(19) -0.006(2) 0.002(2)
C29 0.023(2) 0.031(3) 0.023(2) 0.0026(18) 0.0049(17) -0.0001(19)
C30 0.046(3) 0.027(3) 0.035(3) 0.001(2) 0.008(2) 0.002(2)
C31 0.032(3) 0.036(3) 0.044(3) 0.005(2) -0.001(2) -0.003(2)
C32 0.043(3) 0.049(3) 0.039(3) 0.017(2) 0.008(2) 0.004(2)
C33 0.019(2) 0.025(2) 0.024(2) 0.0022(18) 0.0040(17) 0.0016(18)
C34 0.027(2) 0.029(3) 0.025(2) -0.0009(19) -0.0008(18) 0.0034(19)
C35 0.031(2) 0.033(3) 0.024(2) -0.0002(19) -0.0006(19) 0.009(2)
C36 0.030(2) 0.037(3) 0.029(2) 0.000(2) -0.0013(19) 0.008(2)
N22 0.0243(18) 0.0188(19) 0.0211(17) 0.0032(14) 0.0025(14) 0.0011(15)
C37 0.033(2) 0.017(2) 0.023(2) -0.0009(17) 0.0057(18) -0.0027(18)
C38 0.026(2) 0.026(2) 0.024(2) 0.0002(18) 0.0035(18) -0.0064(19)
C39 0.032(2) 0.028(3) 0.028(2) -0.0061(19) 0.0021(19) -0.002(2)
C40 0.031(2) 0.039(3) 0.029(2) -0.010(2) 0.004(2) -0.006(2)
C41 0.024(2) 0.026(2) 0.024(2) 0.0015(18) -0.0014(17) -0.0002(18)
C42 0.027(2) 0.028(3) 0.042(3) -0.001(2) -0.002(2) 0.004(2)
C43 0.037(3) 0.037(3) 0.042(3) -0.001(2) -0.001(2) 0.014(2)
C44 0.060(4) 0.067(4) 0.072(4) 0.019(3) 0.031(3) 0.031(3)
C45 0.022(2) 0.022(2) 0.025(2) 0.0045(18) 0.0015(17) -0.0044(18)
C46 0.021(2) 0.027(2) 0.036(2) -0.001(2) 0.0030(18) -0.0016(19)
C47 0.028(2) 0.036(3) 0.033(2) -0.005(2) 0.0082(19) -0.006(2)
C48 0.040(3) 0.042(3) 0.056(3) -0.016(3) 0.019(2) -0.013(2)
C49 0.036(2) 0.031(3) 0.016(2) -0.0040(18) -0.0078(18) 0.007(2)
C50 0.067(3) 0.029(3) 0.023(2) 0.006(2) 0.006(2) 0.017(2)
C51 0.127(5) 0.034(3) 0.021(3) -0.001(2) -0.005(3) 0.024(3)
C52 0.215(9) 0.064(5) 0.031(3) 0.014(3) 0.016(4) 0.043(5)
_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
Ni1 O15 2.029(3) . ?
Ni1 N11 2.053(3) . ?
Ni1 N1 2.070(3) . ?
Ni1 O5 2.070(3) . ?
Ni1 O1W 2.102(3) . ?
Ni1 O2W 2.129(3) . ?
N1 C2 1.350(5) . ?
N1 C6 1.370(5) . ?
C2 O2 1.262(5) . ?
C2 N3 1.376(5) . ?
N3 C4 1.380(5) . ?
N3 H3 0.8800 . ?
C4 O4 1.260(4) . ?
C4 C5 1.421(5) . ?
C5 C6 1.343(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.537(5) . ?
O5 C7 1.276(5) . ?
C7 O6 1.231(5) . ?
N11 C12 1.352(5) . ?
N11 C16 1.365(5) . ?
C12 O12 1.259(5) . ?
C12 N13 1.389(5) . ?
N13 C14 1.376(5) . ?
N13 H13 0.8800 . ?
C14 O14 1.249(5) . ?
C14 C15 1.430(6) . ?
C15 C16 1.358(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.530(5) . ?
O15 C17 1.274(5) . ?
C17 O16 1.244(5) . ?
O1W H1WA 0.97(7) . ?
O1W H1WB 0.81(5) . ?
O2W H2WA 0.85(5) . ?
O2W H2WB 0.93(5) . ?
O4W H4A 0.96(6) . ?
O4W H4B 0.96(6) . ?
N21 C25 1.515(5) . ?
N21 C29 1.518(5) . ?
N21 C21 1.527(5) . ?
N21 C33 1.529(5) . ?
C21 C22 1.515(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.529(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.502(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.511(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.525(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.514(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.514(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.530(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.499(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.518(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.526(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.519(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N22 C41 1.512(5) . ?
N22 C45 1.516(5) . ?
N22 C37 1.517(5) . ?
N22 C49 1.526(5) . ?
C37 C38 1.527(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.526(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.523(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.514(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.531(6) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.519(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.512(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.523(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.513(6) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.517(6) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.534(6) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.516(8) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
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
O15 Ni1 N11 81.20(12) . . ?
O15 Ni1 N1 94.52(12) . . ?
N11 Ni1 N1 172.34(13) . . ?
O15 Ni1 O5 91.86(11) . . ?
N11 Ni1 O5 93.80(11) . . ?
N1 Ni1 O5 79.93(11) . . ?
O15 Ni1 O1W 89.39(12) . . ?
N11 Ni1 O1W 92.47(13) . . ?
N1 Ni1 O1W 93.84(13) . . ?
O5 Ni1 O1W 173.72(12) . . ?
O15 Ni1 O2W 173.23(11) . . ?
N11 Ni1 O2W 92.03(13) . . ?
N1 Ni1 O2W 92.22(12) . . ?
O5 Ni1 O2W 88.75(12) . . ?
O1W Ni1 O2W 90.74(13) . . ?
C2 N1 C6 117.1(3) . . ?
C2 N1 Ni1 129.1(3) . . ?
C6 N1 Ni1 113.2(2) . . ?
O2 C2 N1 122.3(3) . . ?
O2 C2 N3 118.7(3) . . ?
N1 C2 N3 118.9(4) . . ?
C2 N3 C4 125.3(3) . . ?
C2 N3 H3 117.4 . . ?
C4 N3 H3 117.4 . . ?
O4 C4 N3 120.1(3) . . ?
O4 C4 C5 125.8(4) . . ?
N3 C4 C5 114.1(3) . . ?
C6 C5 C4 119.0(4) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 N1 125.2(3) . . ?
C5 C6 C7 120.7(4) . . ?
N1 C6 C7 114.1(3) . . ?
C7 O5 Ni1 116.2(2) . . ?
O6 C7 O5 126.8(4) . . ?
O6 C7 C6 117.5(3) . . ?
O5 C7 C6 115.6(4) . . ?
C12 N11 C16 117.7(3) . . ?
C12 N11 Ni1 130.1(3) . . ?
C16 N11 Ni1 111.7(2) . . ?
O12 C12 N11 122.6(4) . . ?
O12 C12 N13 118.3(3) . . ?
N11 C12 N13 119.2(4) . . ?
C14 N13 C12 124.8(3) . . ?
C14 N13 H13 117.6 . . ?
C12 N13 H13 117.6 . . ?
O14 C14 N13 120.0(4) . . ?
O14 C14 C15 125.6(4) . . ?
N13 C14 C15 114.4(4) . . ?
C16 C15 C14 119.3(4) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 N11 124.5(4) . . ?
C15 C16 C17 120.8(4) . . ?
N11 C16 C17 114.8(3) . . ?
C17 O15 Ni1 115.9(2) . . ?
O16 C17 O15 126.2(4) . . ?
O16 C17 C16 118.2(4) . . ?
O15 C17 C16 115.6(4) . . ?
Ni1 O1W H1WA 108(4) . . ?
Ni1 O1W H1WB 110(3) . . ?
H1WA O1W H1WB 112(5) . . ?
Ni1 O2W H2WA 109(4) . . ?
Ni1 O2W H2WB 100(3) . . ?
H2WA O2W H2WB 107(4) . . ?
H4A O4W H4B 102(6) . . ?
C25 N21 C29 106.4(3) . . ?
C25 N21 C21 111.4(3) . . ?
C29 N21 C21 110.9(3) . . ?
C25 N21 C33 111.5(3) . . ?
C29 N21 C33 111.6(3) . . ?
C21 N21 C33 105.1(3) . . ?
C22 C21 N21 115.8(3) . . ?
C22 C21 H21A 108.3 . . ?
N21 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
N21 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 C23 110.8(4) . . ?
C21 C22 H22A 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C24 C23 C22 113.4(4) . . ?
C24 C23 H23A 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N21 115.7(3) . . ?
C26 C25 H25A 108.4 . . ?
N21 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
N21 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 C27 110.2(3) . . ?
C25 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
C25 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
C28 C27 C26 110.6(4) . . ?
C28 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N21 115.9(3) . . ?
C30 C29 H29A 108.3 . . ?
N21 C29 H29A 108.3 . . ?
C30 C29 H29B 108.3 . . ?
N21 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C29 C30 C31 110.0(4) . . ?
C29 C30 H30A 109.7 . . ?
C31 C30 H30A 109.7 . . ?
C29 C30 H30B 109.7 . . ?
C31 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
C32 C31 C30 114.1(4) . . ?
C32 C31 H31A 108.7 . . ?
C30 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C30 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N21 115.5(3) . . ?
C34 C33 H33A 108.4 . . ?
N21 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
N21 C33 H33B 108.4 . . ?
H33A C33 H33B 107.5 . . ?
C33 C34 C35 109.9(3) . . ?
C33 C34 H34A 109.7 . . ?
C35 C34 H34A 109.7 . . ?
C33 C34 H34B 109.7 . . ?
C35 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
C36 C35 C34 111.8(3) . . ?
C36 C35 H35A 109.3 . . ?
C34 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C34 C35 H35B 109.3 . . ?
H35A C35 H35B 107.9 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C41 N22 C45 109.3(3) . . ?
C41 N22 C37 108.6(3) . . ?
C45 N22 C37 111.6(3) . . ?
C41 N22 C49 110.7(3) . . ?
C45 N22 C49 107.6(3) . . ?
C37 N22 C49 109.0(3) . . ?
N22 C37 C38 115.3(3) . . ?
N22 C37 H37A 108.4 . . ?
C38 C37 H37A 108.4 . . ?
N22 C37 H37B 108.4 . . ?
C38 C37 H37B 108.4 . . ?
H37A C37 H37B 107.5 . . ?
C39 C38 C37 111.0(3) . . ?
C39 C38 H38A 109.4 . . ?
C37 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
C37 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
C40 C39 C38 112.4(4) . . ?
C40 C39 H39A 109.1 . . ?
C38 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
C38 C39 H39B 109.1 . . ?
H39A C39 H39B 107.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N22 C41 C42 116.8(3) . . ?
N22 C41 H41A 108.1 . . ?
C42 C41 H41A 108.1 . . ?
N22 C41 H41B 108.1 . . ?
C42 C41 H41B 108.1 . . ?
H41A C41 H41B 107.3 . . ?
C41 C42 C43 110.0(4) . . ?
C41 C42 H42A 109.7 . . ?
C43 C42 H42A 109.7 . . ?
C41 C42 H42B 109.7 . . ?
C43 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
C44 C43 C42 113.7(4) . . ?
C44 C43 H43A 108.8 . . ?
C42 C43 H43A 108.8 . . ?
C44 C43 H43B 108.8 . . ?
C42 C43 H43B 108.8 . . ?
H43A C43 H43B 107.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N22 116.0(3) . . ?
C46 C45 H45A 108.3 . . ?
N22 C45 H45A 108.3 . . ?
C46 C45 H45B 108.3 . . ?
N22 C45 H45B 108.3 . . ?
H45A C45 H45B 107.4 . . ?
C45 C46 C47 109.3(4) . . ?
C45 C46 H46A 109.8 . . ?
C47 C46 H46A 109.8 . . ?
C45 C46 H46B 109.8 . . ?
C47 C46 H46B 109.8 . . ?
H46A C46 H46B 108.3 . . ?
C48 C47 C46 112.3(4) . . ?
C48 C47 H47A 109.2 . . ?
C46 C47 H47A 109.2 . . ?
C48 C47 H47B 109.2 . . ?
C46 C47 H47B 109.2 . . ?
H47A C47 H47B 107.9 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 N22 116.2(3) . . ?
C50 C49 H49A 108.2 . . ?
N22 C49 H49A 108.2 . . ?
C50 C49 H49B 108.2 . . ?
N22 C49 H49B 108.2 . . ?
H49A C49 H49B 107.4 . . ?
C49 C50 C51 107.6(4) . . ?
C49 C50 H50A 110.2 . . ?
C51 C50 H50A 110.2 . . ?
C49 C50 H50B 110.2 . . ?
C51 C50 H50B 110.2 . . ?
H50A C50 H50B 108.5 . . ?
C52 C51 C50 111.9(5) . . ?
C52 C51 H51A 109.2 . . ?
C50 C51 H51A 109.2 . . ?
C52 C51 H51B 109.2 . . ?
C50 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
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
N3 H3 O4 0.88 1.99 2.859(4) 169.9 2_655
N13 H13 O5 0.88 2.08 2.890(4) 153.6 2_756
O1W H1WA O2 0.97(7) 1.81(7) 2.690(4) 150(5) .
O1W H1WB O4W 0.81(5) 1.98(5) 2.760(5) 161(5) .
O2W H2WA O14 0.85(5) 1.94(6) 2.743(4) 158(5) 2_756
O2W H2WB O12 0.93(5) 1.75(5) 2.651(4) 162(4) .
O4W H4A O3W 0.96(6) 2.59(7) 2.725(6) 87(4) 2_656
O4W H4B O12 0.96(6) 1.93(2) 2.885(5) 173(6) .
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 0.828
_refine_diff_density_min -0.451
_refine_diff_density_rms 0.066
# Formatted by publCIF
#===END