# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013
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# 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.
#
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data_lq-1072
_database_code_depnum_ccdc_archive 'CCDC 918640'
#TrackingRef 'LQ-1072.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C18 H12 Ca N6 O3, 0.5(C12 H4 N4)'
_chemical_formula_sum 'C24 H14 Ca N8 O3'
_chemical_formula_weight 502.51
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'
Ca Ca 0.2262 0.3064 '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 9.4930(19)
_cell_length_b 11.242(2)
_cell_length_c 11.270(2)
_cell_angle_alpha 82.89(3)
_cell_angle_beta 83.80(3)
_cell_angle_gamma 77.68(3)
_cell_volume 1161.9(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 7600
_cell_measurement_theta_min 3.16
_cell_measurement_theta_max 27.59
_exptl_crystal_description block
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.11
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.436
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 516
_exptl_absorpt_coefficient_mu 0.315
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8940
_exptl_absorpt_correction_T_max 0.9668
_exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 11395
_diffrn_reflns_av_R_equivalents 0.0758
_diffrn_reflns_av_sigmaI/netI 0.1138
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 3.16
_diffrn_reflns_theta_max 27.48
_reflns_number_total 5253
_reflns_number_gt 2929
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_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^)+(0.0403P)^2^+0.4970P] 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 5253
_refine_ls_number_parameters 325
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1186
_refine_ls_R_factor_gt 0.0615
_refine_ls_wR_factor_ref 0.1545
_refine_ls_wR_factor_gt 0.1206
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_restrained_S_all 1.061
_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
Ca1 Ca 0.97459(8) 0.33006(7) 0.97779(6) 0.0318(2) Uani 1 1 d . . .
C1 C 0.5997(4) 0.3942(3) 0.8485(3) 0.0377(8) Uani 1 1 d . . .
C2 C 0.4813(4) 0.3835(3) 0.7856(3) 0.0332(8) Uani 1 1 d . . .
C3 C 0.3474(4) 0.3771(3) 0.8507(3) 0.0354(8) Uani 1 1 d . . .
C4 C 0.5012(4) 0.3680(3) 0.6604(3) 0.0317(8) Uani 1 1 d . . .
C5 C 0.3885(4) 0.3408(3) 0.6007(3) 0.0351(8) Uani 1 1 d . . .
H5 H 0.3011 0.3334 0.6440 0.042 Uiso 1 1 calc R . .
C6 C 0.4063(4) 0.3254(3) 0.4821(3) 0.0353(8) Uani 1 1 d . . .
H6 H 0.3313 0.3067 0.4459 0.042 Uiso 1 1 calc R . .
C7 C 0.5379(4) 0.3374(3) 0.4120(3) 0.0309(7) Uani 1 1 d . . .
C8 C 0.6499(4) 0.3637(3) 0.4715(3) 0.0352(8) Uani 1 1 d . . .
H8 H 0.7374 0.3711 0.4284 0.042 Uiso 1 1 calc R . .
C9 C 0.6319(4) 0.3785(3) 0.5911(3) 0.0351(8) Uani 1 1 d . . .
H9 H 0.7074 0.3958 0.6277 0.042 Uiso 1 1 calc R . .
C10 C 0.5573(4) 0.3230(3) 0.2879(3) 0.0334(8) Uani 1 1 d . . .
C11 C 0.4436(4) 0.3008(4) 0.2265(3) 0.0401(9) Uani 1 1 d . . .
C12 C 0.6898(4) 0.3266(3) 0.2186(3) 0.0344(8) Uani 1 1 d . . .
C13 C 1.0224(4) 0.3329(3) 0.4503(3) 0.0361(8) Uani 1 1 d . . .
C14 C 1.0162(4) 0.2395(3) 0.5443(3) 0.0342(8) Uani 1 1 d . . .
C15 C 1.0133(4) 0.2710(3) 0.6626(3) 0.0356(8) Uani 1 1 d . . .
C16 C 1.0069(4) 0.0894(3) 0.4039(3) 0.0364(8) Uani 1 1 d . . .
H16 H 1.0113 0.1496 0.3399 0.044 Uiso 1 1 calc R . .
C17 C 1.0081(4) 0.1188(3) 0.5229(3) 0.0337(8) Uani 1 1 d . . .
C18 C 1.0006(4) 0.0248(3) 0.6176(3) 0.0351(8) Uani 1 1 d . . .
H18 H 1.0008 0.0418 0.6962 0.042 Uiso 1 1 calc R . .
C19 C 0.6045(5) 0.0712(4) 0.7910(4) 0.0537(11) Uani 1 1 d . . .
C20 C 0.4874(4) 0.0396(4) 0.7443(3) 0.0428(9) Uani 1 1 d . . .
C21 C 0.3638(6) 0.0282(4) 0.8230(4) 0.0591(12) Uani 1 1 d . . .
C22 C 0.6164(4) 0.0328(4) 0.5424(3) 0.0410(9) Uani 1 1 d . . .
H22 H 0.6946 0.0550 0.5706 0.049 Uiso 1 1 calc R . .
C23 C 0.4948(4) 0.0191(3) 0.6223(3) 0.0388(8) Uani 1 1 d . . .
C24 C 0.3781(4) -0.0143(4) 0.5754(3) 0.0453(10) Uani 1 1 d . . .
H24 H 0.2962 -0.0239 0.6258 0.054 Uiso 1 1 calc R . .
N1 N 0.6997(4) 0.3992(3) 0.8969(3) 0.0455(8) Uani 1 1 d . . .
N2 N 0.2359(3) 0.3707(3) 0.8982(3) 0.0456(8) Uani 1 1 d . . .
N3 N 0.3499(4) 0.2839(4) 0.1797(3) 0.0595(10) Uani 1 1 d . . .
N4 N 0.7985(3) 0.3273(3) 0.1611(3) 0.0451(8) Uani 1 1 d . . .
N5 N 1.0100(4) 0.2956(3) 0.7592(3) 0.0419(8) Uani 1 1 d . . .
N6 N 1.0258(4) 0.4057(3) 0.3698(3) 0.0536(9) Uani 1 1 d . . .
N7 N 0.7018(5) 0.0977(4) 0.8257(4) 0.0757(13) Uani 1 1 d . . .
N8 N 0.2604(6) 0.0174(5) 0.8829(4) 0.0941(16) Uani 1 1 d . . .
O1 O 0.9336(2) 0.5451(2) 0.88556(18) 0.0320(5) Uani 1 1 d . . .
H101 H 0.9828 0.5422 0.8179 0.048 Uiso 1 1 d R . .
H102 H 0.8486 0.5842 0.8729 0.048 Uiso 1 1 d R . .
O2 O 0.9065(3) 0.1424(2) 0.9680(2) 0.0472(7) Uani 1 1 d . . .
H201 H 0.8337 0.1438 0.9296 0.071 Uiso 1 1 d R . .
H202 H 0.9068 0.0834 1.0230 0.071 Uiso 1 1 d R . .
O3 O 1.1337(3) 0.1787(2) 1.0945(2) 0.0496(7) Uani 1 1 d . . .
H301 H 1.1762 0.1125 1.0661 0.074 Uiso 1 1 d R . .
H302 H 1.1944 0.2154 1.1166 0.074 Uiso 1 1 d 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
Ca1 0.0383(4) 0.0392(4) 0.0214(3) -0.0061(3) 0.0027(3) -0.0166(3)
C1 0.041(2) 0.046(2) 0.0261(17) -0.0054(16) 0.0037(16) -0.0121(18)
C2 0.0307(18) 0.046(2) 0.0238(16) -0.0048(15) 0.0022(14) -0.0120(17)
C3 0.037(2) 0.047(2) 0.0236(16) -0.0067(15) 0.0003(15) -0.0118(17)
C4 0.0301(18) 0.039(2) 0.0266(16) -0.0052(14) 0.0016(14) -0.0091(16)
C5 0.0281(18) 0.052(2) 0.0266(17) -0.0046(16) 0.0057(14) -0.0142(17)
C6 0.0254(18) 0.052(2) 0.0325(18) -0.0069(16) -0.0003(14) -0.0164(17)
C7 0.0317(19) 0.037(2) 0.0236(16) -0.0049(14) 0.0007(14) -0.0062(16)
C8 0.0270(17) 0.054(2) 0.0276(17) -0.0080(16) 0.0043(14) -0.0161(17)
C9 0.0270(18) 0.054(2) 0.0272(17) -0.0066(16) -0.0003(14) -0.0138(17)
C10 0.0309(18) 0.047(2) 0.0258(16) -0.0094(15) -0.0002(14) -0.0139(17)
C11 0.041(2) 0.052(2) 0.0266(17) -0.0091(16) 0.0011(16) -0.0080(19)
C12 0.037(2) 0.045(2) 0.0216(16) -0.0069(15) -0.0016(15) -0.0060(17)
C13 0.038(2) 0.046(2) 0.0266(17) -0.0066(16) 0.0009(15) -0.0139(18)
C14 0.0336(19) 0.046(2) 0.0229(16) -0.0070(15) 0.0015(14) -0.0091(17)
C15 0.0349(19) 0.043(2) 0.0313(18) -0.0063(16) 0.0001(15) -0.0136(17)
C16 0.041(2) 0.045(2) 0.0246(16) -0.0057(15) 0.0010(15) -0.0123(18)
C17 0.0271(17) 0.048(2) 0.0276(17) -0.0103(15) 0.0022(14) -0.0100(16)
C18 0.039(2) 0.049(2) 0.0196(15) -0.0064(15) -0.0010(14) -0.0115(17)
C19 0.067(3) 0.048(3) 0.048(2) -0.013(2) -0.012(2) -0.009(2)
C20 0.049(2) 0.043(2) 0.036(2) -0.0017(17) -0.0041(18) -0.0113(19)
C21 0.074(3) 0.058(3) 0.043(2) -0.003(2) 0.000(2) -0.014(3)
C22 0.033(2) 0.048(2) 0.047(2) -0.0088(18) -0.0074(17) -0.0146(18)
C23 0.034(2) 0.037(2) 0.047(2) -0.0057(16) -0.0044(17) -0.0095(17)
C24 0.033(2) 0.059(3) 0.047(2) -0.0095(19) 0.0050(17) -0.018(2)
N1 0.0423(19) 0.067(2) 0.0316(16) -0.0019(15) -0.0054(14) -0.0207(18)
N2 0.0421(19) 0.069(2) 0.0290(16) -0.0104(15) 0.0052(14) -0.0184(18)
N3 0.051(2) 0.089(3) 0.047(2) -0.0202(19) -0.0096(17) -0.023(2)
N4 0.0365(18) 0.065(2) 0.0339(17) -0.0137(16) 0.0047(14) -0.0108(17)
N5 0.053(2) 0.045(2) 0.0314(16) -0.0096(14) 0.0032(14) -0.0185(16)
N6 0.070(3) 0.058(2) 0.0365(18) -0.0062(17) 0.0027(17) -0.023(2)
N7 0.081(3) 0.079(3) 0.075(3) -0.024(2) -0.032(2) -0.013(3)
N8 0.098(4) 0.117(4) 0.066(3) -0.004(3) 0.026(3) -0.038(3)
O1 0.0348(13) 0.0387(14) 0.0237(11) -0.0061(10) -0.0007(10) -0.0090(11)
O2 0.0525(17) 0.0493(17) 0.0486(15) -0.0016(13) -0.0146(13) -0.0262(14)
O3 0.0486(17) 0.0436(17) 0.0595(17) -0.0083(13) -0.0132(14) -0.0099(14)
_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
Ca1 O2 2.353(2) . ?
Ca1 O3 2.384(3) . ?
Ca1 O1 2.478(2) . ?
Ca1 N4 2.515(3) 1_556 ?
Ca1 N5 2.517(3) . ?
Ca1 O1 2.539(2) 2_767 ?
Ca1 N2 2.659(3) 1_655 ?
Ca1 N1 2.778(3) . ?
Ca1 Ca1 4.0492(16) 2_767 ?
Ca1 H302 2.7425 . ?
C1 N1 1.159(4) . ?
C1 C2 1.426(5) . ?
C2 C3 1.408(5) . ?
C2 C4 1.431(4) . ?
C3 N2 1.145(4) . ?
C4 C9 1.411(4) . ?
C4 C5 1.428(4) . ?
C5 C6 1.356(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.427(4) . ?
C6 H6 0.9300 . ?
C7 C10 1.416(4) . ?
C7 C8 1.416(4) . ?
C8 C9 1.366(4) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C12 1.413(5) . ?
C10 C11 1.423(5) . ?
C11 N3 1.142(4) . ?
C12 N4 1.158(4) . ?
C13 N6 1.147(4) . ?
C13 C14 1.402(5) . ?
C14 C15 1.417(4) . ?
C14 C17 1.426(5) . ?
C15 N5 1.152(4) . ?
C16 C18 1.353(5) 2_756 ?
C16 C17 1.422(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.414(5) . ?
C18 C16 1.353(5) 2_756 ?
C18 H18 0.9300 . ?
C19 N7 1.149(5) . ?
C19 C20 1.407(6) . ?
C20 C21 1.411(6) . ?
C20 C23 1.414(5) . ?
C21 N8 1.150(6) . ?
C22 C24 1.362(5) 2_656 ?
C22 C23 1.409(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.415(5) . ?
C24 C22 1.362(5) 2_656 ?
C24 H24 0.9300 . ?
N2 Ca1 2.659(3) 1_455 ?
N4 Ca1 2.515(3) 1_554 ?
O1 Ca1 2.539(2) 2_767 ?
O1 H101 0.8499 . ?
O1 H102 0.8500 . ?
O2 H201 0.8500 . ?
O2 H202 0.8500 . ?
O3 H301 0.8500 . ?
O3 H302 0.8500 . ?
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
O2 Ca1 O3 73.52(9) . . ?
O2 Ca1 O1 141.72(8) . . ?
O3 Ca1 O1 143.67(8) . . ?
O2 Ca1 N4 80.16(10) . 1_556 ?
O3 Ca1 N4 85.20(11) . 1_556 ?
O1 Ca1 N4 105.92(10) . 1_556 ?
O2 Ca1 N5 74.42(10) . . ?
O3 Ca1 N5 111.70(11) . . ?
O1 Ca1 N5 80.05(9) . . ?
N4 Ca1 N5 143.30(10) 1_556 . ?
O2 Ca1 O1 143.78(9) . 2_767 ?
O3 Ca1 O1 76.93(8) . 2_767 ?
O1 Ca1 O1 72.38(8) . 2_767 ?
N4 Ca1 O1 76.92(9) 1_556 2_767 ?
N5 Ca1 O1 137.26(9) . 2_767 ?
O2 Ca1 N2 122.78(11) . 1_655 ?
O3 Ca1 N2 76.26(10) . 1_655 ?
O1 Ca1 N2 74.64(10) . 1_655 ?
N4 Ca1 N2 143.26(9) 1_556 1_655 ?
N5 Ca1 N2 73.43(10) . 1_655 ?
O1 Ca1 N2 68.20(9) 2_767 1_655 ?
O2 Ca1 N1 76.40(10) . . ?
O3 Ca1 N1 145.62(10) . . ?
O1 Ca1 N1 69.68(9) . . ?
N4 Ca1 N1 73.55(10) 1_556 . ?
N5 Ca1 N1 75.03(10) . . ?
O1 Ca1 N1 122.14(10) 2_767 . ?
N2 Ca1 N1 135.54(10) 1_655 . ?
O2 Ca1 Ca1 170.48(8) . 2_767 ?
O3 Ca1 Ca1 110.56(7) . 2_767 ?
O1 Ca1 Ca1 36.71(5) . 2_767 ?
N4 Ca1 Ca1 91.48(8) 1_556 2_767 ?
N5 Ca1 Ca1 110.78(8) . 2_767 ?
O1 Ca1 Ca1 35.68(5) 2_767 2_767 ?
N2 Ca1 Ca1 66.73(8) 1_655 2_767 ?
N1 Ca1 Ca1 96.96(8) . 2_767 ?
O2 Ca1 H302 90.8 . . ?
O3 Ca1 H302 17.3 . . ?
O1 Ca1 H302 126.4 . . ?
N4 Ca1 H302 89.4 1_556 . ?
N5 Ca1 H302 116.7 . . ?
O1 Ca1 H302 61.5 2_767 . ?
N2 Ca1 H302 64.4 1_655 . ?
N1 Ca1 H302 160.0 . . ?
Ca1 Ca1 H302 93.7 2_767 . ?
N1 C1 C2 177.1(4) . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 C4 120.2(3) . . ?
C1 C2 C4 120.6(3) . . ?
N2 C3 C2 176.3(4) . . ?
C9 C4 C5 117.4(3) . . ?
C9 C4 C2 121.9(3) . . ?
C5 C4 C2 120.8(3) . . ?
C6 C5 C4 121.3(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 121.2(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C10 C7 C8 120.9(3) . . ?
C10 C7 C6 121.7(3) . . ?
C8 C7 C6 117.4(3) . . ?
C9 C8 C7 121.3(3) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C4 121.5(3) . . ?
C8 C9 H9 119.3 . . ?
C4 C9 H9 119.3 . . ?
C12 C10 C7 122.6(3) . . ?
C12 C10 C11 116.2(3) . . ?
C7 C10 C11 121.2(3) . . ?
N3 C11 C10 178.3(4) . . ?
N4 C12 C10 178.7(4) . . ?
N6 C13 C14 176.7(4) . . ?
C13 C14 C15 117.1(3) . . ?
C13 C14 C17 121.8(3) . . ?
C15 C14 C17 121.1(3) . . ?
N5 C15 C14 179.2(4) . . ?
C18 C16 C17 121.0(3) 2_756 . ?
C18 C16 H16 119.5 2_756 . ?
C17 C16 H16 119.5 . . ?
C18 C17 C16 117.6(3) . . ?
C18 C17 C14 121.9(3) . . ?
C16 C17 C14 120.5(3) . . ?
C16 C18 C17 121.4(3) 2_756 . ?
C16 C18 H18 119.3 2_756 . ?
C17 C18 H18 119.3 . . ?
N7 C19 C20 178.0(5) . . ?
C19 C20 C21 118.0(4) . . ?
C19 C20 C23 120.6(4) . . ?
C21 C20 C23 121.4(4) . . ?
N8 C21 C20 177.0(5) . . ?
C24 C22 C23 121.5(3) 2_656 . ?
C24 C22 H22 119.3 2_656 . ?
C23 C22 H22 119.3 . . ?
C22 C23 C20 121.9(3) . . ?
C22 C23 C24 117.3(3) . . ?
C20 C23 C24 120.8(3) . . ?
C22 C24 C23 121.2(3) 2_656 . ?
C22 C24 H24 119.4 2_656 . ?
C23 C24 H24 119.4 . . ?
C1 N1 Ca1 158.9(3) . . ?
C3 N2 Ca1 169.6(3) . 1_455 ?
C12 N4 Ca1 159.1(3) . 1_554 ?
C15 N5 Ca1 171.4(3) . . ?
Ca1 O1 Ca1 107.62(8) . 2_767 ?
Ca1 O1 H101 104.6 . . ?
Ca1 O1 H101 112.1 2_767 . ?
Ca1 O1 H102 120.5 . . ?
Ca1 O1 H102 104.9 2_767 . ?
H101 O1 H102 107.2 . . ?
Ca1 O2 H201 117.5 . . ?
Ca1 O2 H202 127.7 . . ?
H201 O2 H202 105.4 . . ?
Ca1 O3 H301 120.2 . . ?
Ca1 O3 H302 105.9 . . ?
H301 O3 H302 111.0 . . ?
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
O1 H101 N6 0.85 2.13 2.863(4) 144.2 2_766
O1 H102 N3 0.85 2.22 3.058(5) 168.1 2_666
O2 H201 N7 0.85 1.99 2.808(4) 162.0 .
O2 H202 N8 0.85 2.24 2.908(5) 135.0 2_657
O3 H301 N7 0.85 2.61 3.232(5) 130.5 2_757
O3 H302 N3 0.85 2.03 2.877(4) 173.2 1_656
_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full 27.48
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max 0.360
_refine_diff_density_min -0.572
_refine_diff_density_rms 0.075
data_lq-98-2
_database_code_depnum_ccdc_archive 'CCDC 918641'
#TrackingRef 'LQ-98-2.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C18 H12 Ba N6 O3, 0.5(C12 H4 N4)'
_chemical_formula_sum 'C24 H14 Ba N8 O3'
_chemical_formula_weight 599.77
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'
Ba Ba -0.3244 2.2819 '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'
_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 9.809(5)
_cell_length_b 11.058(5)
_cell_length_c 11.698(6)
_cell_angle_alpha 81.23(2)
_cell_angle_beta 81.570(19)
_cell_angle_gamma 81.25(2)
_cell_volume 1229.5(10)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 11038
_cell_measurement_theta_min 3.01
_cell_measurement_theta_max 27.55
_exptl_crystal_description block
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.620
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 588
_exptl_absorpt_coefficient_mu 1.657
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6477
_exptl_absorpt_correction_T_max 0.7296
_exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 12142
_diffrn_reflns_av_R_equivalents 0.0188
_diffrn_reflns_av_sigmaI/netI 0.0249
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 3.01
_diffrn_reflns_theta_max 27.48
_reflns_number_total 5585
_reflns_number_gt 5048
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_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^)+(0.0486P)^2^+0.0947P] 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 5585
_refine_ls_number_parameters 325
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0286
_refine_ls_R_factor_gt 0.0241
_refine_ls_wR_factor_ref 0.0771
_refine_ls_wR_factor_gt 0.0701
_refine_ls_goodness_of_fit_ref 1.135
_refine_ls_restrained_S_all 1.135
_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
Ba1 Ba 0.941372(15) 0.324667(13) 0.995486(11) 0.03182(7) Uani 1 1 d . . .
C1 C 0.5745(3) 0.3939(3) 0.8548(2) 0.0401(6) Uani 1 1 d . . .
C2 C 0.4578(3) 0.3975(3) 0.7942(2) 0.0367(6) Uani 1 1 d . . .
C3 C 0.3247(3) 0.4189(3) 0.8585(2) 0.0374(6) Uani 1 1 d . . .
C4 C 0.4723(3) 0.3733(2) 0.6768(2) 0.0320(5) Uani 1 1 d . . .
C5 C 0.3553(3) 0.3686(3) 0.6206(2) 0.0373(6) Uani 1 1 d . . .
H5 H 0.2668 0.3822 0.6613 0.045 Uiso 1 1 calc R . .
C6 C 0.3689(3) 0.3447(3) 0.5079(2) 0.0386(6) Uani 1 1 d . . .
H6 H 0.2897 0.3429 0.4734 0.046 Uiso 1 1 calc R . .
C7 C 0.5021(3) 0.3227(3) 0.4428(2) 0.0346(5) Uani 1 1 d . . .
C8 C 0.6181(3) 0.3269(3) 0.4998(3) 0.0419(6) Uani 1 1 d . . .
H8 H 0.7068 0.3132 0.4593 0.050 Uiso 1 1 calc R . .
C9 C 0.6046(3) 0.3504(3) 0.6118(3) 0.0410(6) Uani 1 1 d . . .
H9 H 0.6840 0.3514 0.6463 0.049 Uiso 1 1 calc R . .
C10 C 0.5185(3) 0.2985(3) 0.3259(2) 0.0367(6) Uani 1 1 d . . .
C11 C 0.4041(3) 0.2902(3) 0.2686(3) 0.0458(7) Uani 1 1 d . . .
C12 C 0.6505(3) 0.2805(3) 0.2597(2) 0.0409(6) Uani 1 1 d . . .
C13 C 0.9788(3) 0.3461(3) 0.4600(2) 0.0358(6) Uani 1 1 d . . .
C14 C 0.9859(3) 0.2452(2) 0.5493(2) 0.0315(5) Uani 1 1 d . . .
C15 C 0.9806(3) 0.2720(2) 0.6645(2) 0.0363(6) Uani 1 1 d . . .
C16 C 0.9959(3) 0.0970(2) 0.4087(2) 0.0334(5) Uani 1 1 d . . .
H16 H 0.9931 0.1620 0.3481 0.040 Uiso 1 1 calc R . .
C17 C 0.9926(2) 0.1220(2) 0.5256(2) 0.0292(5) Uani 1 1 d . . .
C18 C 0.9970(3) 0.0204(2) 0.6151(2) 0.0341(5) Uani 1 1 d . . .
H18 H 0.9949 0.0342 0.6918 0.041 Uiso 1 1 calc R . .
C19 C 0.5863(5) 0.0674(4) 0.7859(5) 0.0778(13) Uani 1 1 d . . .
C20 C 0.4699(5) 0.0596(3) 0.7293(5) 0.0738(13) Uani 1 1 d . . .
C21 C 0.3367(6) 0.0857(5) 0.7964(5) 0.0899(17) Uani 1 1 d . . .
C22 C 0.6171(4) 0.0048(3) 0.5497(5) 0.0762(14) Uani 1 1 d . . .
H22 H 0.6965 0.0085 0.5832 0.091 Uiso 1 1 calc R . .
C23 C 0.4852(4) 0.0301(3) 0.6151(4) 0.0676(12) Uani 1 1 d . . .
C24 C 0.3685(4) 0.0243(3) 0.5584(5) 0.0722(12) Uani 1 1 d . . .
H24 H 0.2797 0.0411 0.5977 0.087 Uiso 1 1 calc R . .
N1 N 0.6680(3) 0.3903(3) 0.9024(3) 0.0570(7) Uani 1 1 d . . .
N2 N 0.2160(3) 0.4353(3) 0.9088(2) 0.0495(7) Uani 1 1 d . . .
N3 N 0.3103(3) 0.2852(4) 0.2225(3) 0.0697(9) Uani 1 1 d . . .
N4 N 0.7570(3) 0.2681(3) 0.2057(2) 0.0582(8) Uani 1 1 d . . .
N5 N 0.9748(3) 0.2934(2) 0.7575(2) 0.0528(7) Uani 1 1 d . . .
N6 N 0.9708(3) 0.4259(3) 0.3852(2) 0.0555(7) Uani 1 1 d . . .
N7 N 0.6782(5) 0.0737(4) 0.8314(5) 0.1005(16) Uani 1 1 d . . .
N8 N 0.2306(6) 0.1062(6) 0.8488(5) 0.128(2) Uani 1 1 d . . .
O1 O 0.93551(19) 0.55422(17) 0.85595(15) 0.0347(4) Uani 1 1 d . . .
H101 H 0.9837 0.5514 0.7896 0.052 Uiso 1 1 d R . .
H102 H 0.8553 0.5912 0.8440 0.052 Uiso 1 1 d R . .
O2 O 0.8708(3) 0.1017(2) 0.9810(2) 0.0599(6) Uani 1 1 d . . .
H201 H 0.8017 0.1030 0.9445 0.090 Uiso 1 1 d R . .
H202 H 0.8712 0.0422 1.0364 0.090 Uiso 1 1 d R . .
O3 O 1.1244(3) 0.1649(2) 1.1178(3) 0.0753(8) Uani 1 1 d . . .
H301 H 1.1658 0.1004 1.0901 0.113 Uiso 1 1 d R . .
H302 H 1.1845 0.2013 1.1397 0.113 Uiso 1 1 d 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
Ba1 0.04105(10) 0.03743(10) 0.02087(8) -0.00215(6) -0.00803(6) -0.01523(6)
C1 0.0335(13) 0.0513(16) 0.0377(14) -0.0173(13) -0.0034(11) -0.0024(11)
C2 0.0274(12) 0.0472(15) 0.0371(14) -0.0152(12) -0.0024(10) -0.0019(11)
C3 0.0331(13) 0.0482(15) 0.0323(13) -0.0127(12) -0.0059(10) -0.0009(11)
C4 0.0265(11) 0.0381(13) 0.0323(12) -0.0078(11) -0.0061(10) -0.0016(10)
C5 0.0248(11) 0.0504(16) 0.0362(13) -0.0101(12) -0.0044(10) 0.0012(11)
C6 0.0253(12) 0.0528(16) 0.0399(14) -0.0109(13) -0.0109(10) -0.0012(11)
C7 0.0327(13) 0.0363(13) 0.0353(13) -0.0089(11) -0.0034(10) -0.0035(10)
C8 0.0255(12) 0.0615(18) 0.0414(15) -0.0186(14) 0.0024(11) -0.0094(11)
C9 0.0240(12) 0.0612(18) 0.0423(15) -0.0192(14) -0.0061(11) -0.0060(11)
C10 0.0367(13) 0.0406(14) 0.0334(13) -0.0085(11) -0.0066(11) -0.0019(11)
C11 0.0467(16) 0.0539(18) 0.0379(15) -0.0128(14) -0.0119(13) 0.0028(13)
C12 0.0461(16) 0.0481(16) 0.0285(13) -0.0052(12) -0.0070(12) -0.0039(12)
C13 0.0427(14) 0.0389(14) 0.0273(12) -0.0102(11) -0.0010(10) -0.0078(11)
C14 0.0346(12) 0.0355(13) 0.0243(11) -0.0069(10) -0.0008(9) -0.0041(10)
C15 0.0441(14) 0.0330(13) 0.0317(13) -0.0088(11) 0.0002(11) -0.0051(11)
C16 0.0417(14) 0.0371(13) 0.0208(11) -0.0025(10) -0.0032(10) -0.0053(11)
C17 0.0287(11) 0.0352(12) 0.0241(11) -0.0088(10) -0.0007(9) -0.0027(9)
C18 0.0414(13) 0.0392(14) 0.0219(11) -0.0095(10) -0.0002(10) -0.0040(11)
C19 0.088(3) 0.048(2) 0.110(4) -0.006(2) -0.065(3) -0.0029(19)
C20 0.079(3) 0.0457(19) 0.107(4) 0.011(2) -0.060(3) -0.0160(18)
C21 0.098(4) 0.082(3) 0.097(4) 0.039(3) -0.048(3) -0.048(3)
C22 0.055(2) 0.0503(19) 0.138(4) -0.011(2) -0.061(3) -0.0080(16)
C23 0.066(2) 0.0372(16) 0.111(3) 0.0049(19) -0.058(2) -0.0105(15)
C24 0.056(2) 0.055(2) 0.118(4) -0.007(2) -0.055(2) -0.0105(17)
N1 0.0391(14) 0.084(2) 0.0550(16) -0.0271(16) -0.0131(12) -0.0054(13)
N2 0.0343(12) 0.0777(19) 0.0354(12) -0.0151(13) -0.0024(10) 0.0015(12)
N3 0.0577(18) 0.095(2) 0.0628(19) -0.0214(18) -0.0318(16) 0.0047(17)
N4 0.0525(16) 0.081(2) 0.0381(14) -0.0092(14) 0.0051(12) -0.0070(14)
N5 0.086(2) 0.0433(14) 0.0304(12) -0.0115(11) -0.0065(12) -0.0058(13)
N6 0.085(2) 0.0477(15) 0.0335(13) -0.0022(12) -0.0037(13) -0.0137(14)
N7 0.103(3) 0.078(2) 0.140(4) -0.030(3) -0.078(3) 0.003(2)
N8 0.101(4) 0.180(6) 0.100(4) 0.051(4) -0.020(3) -0.070(4)
O1 0.0378(9) 0.0410(10) 0.0263(8) -0.0063(8) -0.0089(7) -0.0014(8)
O2 0.0774(16) 0.0479(12) 0.0618(15) 0.0005(11) -0.0256(13) -0.0240(12)
O3 0.0761(18) 0.0511(14) 0.100(2) -0.0217(15) -0.0295(16) 0.0161(13)
_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
Ba1 O2 2.696(2) . ?
Ba1 O3 2.722(3) . ?
Ba1 O1 2.798(2) . ?
Ba1 N5 2.823(3) . ?
Ba1 O1 2.844(2) 2_767 ?
Ba1 N4 2.878(3) 1_556 ?
Ba1 N1 2.987(3) . ?
Ba1 N2 3.099(3) 1_655 ?
Ba1 N2 3.137(3) 2_667 ?
C1 N1 1.134(4) . ?
C1 C2 1.424(4) . ?
C2 C3 1.414(4) . ?
C2 C4 1.422(4) . ?
C3 N2 1.143(4) . ?
C4 C9 1.413(4) . ?
C4 C5 1.415(4) . ?
C5 C6 1.367(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.420(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.410(4) . ?
C7 C10 1.415(4) . ?
C8 C9 1.358(4) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.410(4) . ?
C10 C12 1.410(4) . ?
C11 N3 1.144(4) . ?
C12 N4 1.140(4) . ?
C13 N6 1.147(4) . ?
C13 C14 1.409(4) . ?
C14 C15 1.416(3) . ?
C14 C17 1.420(4) . ?
C15 N5 1.140(4) . ?
C16 C18 1.358(4) 2_756 ?
C16 C17 1.431(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.414(4) . ?
C18 C16 1.358(4) 2_756 ?
C18 H18 0.9300 . ?
C19 N7 1.129(5) . ?
C19 C20 1.420(5) . ?
C20 C23 1.405(7) . ?
C20 C21 1.436(8) . ?
C21 N8 1.137(8) . ?
C22 C24 1.335(7) 2_656 ?
C22 C23 1.415(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.419(5) . ?
C24 C22 1.335(7) 2_656 ?
C24 H24 0.9300 . ?
N2 Ba1 3.099(3) 1_455 ?
N2 Ba1 3.137(3) 2_667 ?
N4 Ba1 2.878(3) 1_554 ?
O1 Ba1 2.844(2) 2_767 ?
O1 H101 0.8499 . ?
O1 H102 0.8500 . ?
O2 H201 0.8500 . ?
O2 H202 0.8500 . ?
O3 H301 0.8500 . ?
O3 H302 0.8500 . ?
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
O2 Ba1 O3 76.60(9) . . ?
O2 Ba1 O1 136.50(7) . . ?
O3 Ba1 O1 138.02(8) . . ?
O2 Ba1 N5 72.08(8) . . ?
O3 Ba1 N5 112.63(9) . . ?
O1 Ba1 N5 69.78(7) . . ?
O2 Ba1 O1 140.55(7) . 2_767 ?
O3 Ba1 O1 68.27(8) . 2_767 ?
O1 Ba1 O1 82.90(6) . 2_767 ?
N5 Ba1 O1 138.05(8) . 2_767 ?
O2 Ba1 N4 75.00(9) . 1_556 ?
O3 Ba1 N4 81.46(10) . 1_556 ?
O1 Ba1 N4 125.46(8) . 1_556 ?
N5 Ba1 N4 139.40(10) . 1_556 ?
O1 Ba1 N4 82.42(8) 2_767 1_556 ?
O2 Ba1 N1 77.46(9) . . ?
O3 Ba1 N1 151.30(10) . . ?
O1 Ba1 N1 70.58(8) . . ?
N5 Ba1 N1 70.12(9) . . ?
O1 Ba1 N1 130.14(7) 2_767 . ?
N4 Ba1 N1 80.15(9) 1_556 . ?
O2 Ba1 N2 130.81(8) . 1_655 ?
O3 Ba1 N2 78.56(9) . 1_655 ?
O1 Ba1 N2 60.26(7) . 1_655 ?
N5 Ba1 N2 79.52(8) . 1_655 ?
O1 Ba1 N2 59.11(6) 2_767 1_655 ?
N4 Ba1 N2 140.98(8) 1_556 1_655 ?
N1 Ba1 N2 128.63(9) . 1_655 ?
O2 Ba1 N2 134.56(8) . 2_667 ?
O3 Ba1 N2 121.57(8) . 2_667 ?
O1 Ba1 N2 59.06(7) . 2_667 ?
N5 Ba1 N2 123.07(8) . 2_667 ?
O1 Ba1 N2 59.35(7) 2_767 2_667 ?
N4 Ba1 N2 68.31(9) 1_556 2_667 ?
N1 Ba1 N2 70.79(8) . 2_667 ?
N2 Ba1 N2 94.59(7) 1_655 2_667 ?
O2 Ba1 Ba1 177.78(6) . 2_767 ?
O3 Ba1 Ba1 104.06(7) . 2_767 ?
O1 Ba1 Ba1 41.86(4) . 2_767 ?
N5 Ba1 Ba1 105.75(6) . 2_767 ?
O1 Ba1 Ba1 41.04(4) 2_767 2_767 ?
N4 Ba1 Ba1 107.17(7) 1_556 2_767 ?
N1 Ba1 Ba1 102.33(7) . 2_767 ?
N2 Ba1 Ba1 47.67(5) 1_655 2_767 ?
N2 Ba1 Ba1 46.92(6) 2_667 2_767 ?
N1 C1 C2 179.4(3) . . ?
C3 C2 C4 120.6(2) . . ?
C3 C2 C1 116.9(2) . . ?
C4 C2 C1 122.4(2) . . ?
N2 C3 C2 178.6(3) . . ?
C9 C4 C5 117.0(2) . . ?
C9 C4 C2 121.4(2) . . ?
C5 C4 C2 121.6(2) . . ?
C6 C5 C4 121.8(2) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C7 120.9(2) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C10 121.3(2) . . ?
C8 C7 C6 116.9(2) . . ?
C10 C7 C6 121.8(3) . . ?
C9 C8 C7 122.2(2) . . ?
C9 C8 H8 118.9 . . ?
C7 C8 H8 118.9 . . ?
C8 C9 C4 121.2(3) . . ?
C8 C9 H9 119.4 . . ?
C4 C9 H9 119.4 . . ?
C11 C10 C12 115.9(3) . . ?
C11 C10 C7 122.1(3) . . ?
C12 C10 C7 122.0(3) . . ?
N3 C11 C10 179.0(4) . . ?
N4 C12 C10 178.8(4) . . ?
N6 C13 C14 177.7(3) . . ?
C13 C14 C15 117.1(2) . . ?
C13 C14 C17 121.5(2) . . ?
C15 C14 C17 121.3(2) . . ?
N5 C15 C14 179.2(3) . . ?
C18 C16 C17 121.0(2) 2_756 . ?
C18 C16 H16 119.5 2_756 . ?
C17 C16 H16 119.5 . . ?
C18 C17 C14 121.9(2) . . ?
C18 C17 C16 117.6(2) . . ?
C14 C17 C16 120.4(2) . . ?
C16 C18 C17 121.4(2) 2_756 . ?
C16 C18 H18 119.3 2_756 . ?
C17 C18 H18 119.3 . . ?
N7 C19 C20 179.6(7) . . ?
C23 C20 C19 121.9(5) . . ?
C23 C20 C21 122.8(4) . . ?
C19 C20 C21 115.3(5) . . ?
N8 C21 C20 179.4(7) . . ?
C24 C22 C23 122.2(3) 2_656 . ?
C24 C22 H22 118.9 2_656 . ?
C23 C22 H22 118.9 . . ?
C20 C23 C22 122.3(4) . . ?
C20 C23 C24 121.6(4) . . ?
C22 C23 C24 116.1(4) . . ?
C22 C24 C23 121.8(4) 2_656 . ?
C22 C24 H24 119.1 2_656 . ?
C23 C24 H24 119.1 . . ?
C1 N1 Ba1 165.2(2) . . ?
C3 N2 Ba1 145.0(3) . 1_455 ?
C3 N2 Ba1 129.4(3) . 2_667 ?
Ba1 N2 Ba1 85.41(7) 1_455 2_667 ?
C12 N4 Ba1 150.9(3) . 1_554 ?
C15 N5 Ba1 173.5(3) . . ?
Ba1 O1 Ba1 97.10(6) . 2_767 ?
Ba1 O1 H101 113.4 . . ?
Ba1 O1 H101 112.2 2_767 . ?
Ba1 O1 H102 115.8 . . ?
Ba1 O1 H102 111.3 2_767 . ?
H101 O1 H102 107.0 . . ?
Ba1 O2 H201 115.3 . . ?
Ba1 O2 H202 124.1 . . ?
H201 O2 H202 109.5 . . ?
Ba1 O3 H301 119.9 . . ?
Ba1 O3 H302 112.2 . . ?
H301 O3 H302 108.5 . . ?
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
O1 H101 N6 0.85 2.01 2.821(3) 158.6 2_766
O1 H102 N3 0.85 2.12 2.943(4) 163.6 2_666
O2 H201 N7 0.85 2.01 2.835(4) 163.4 .
O2 H202 N8 0.85 2.22 2.994(6) 151.3 2_657
O3 H301 N7 0.85 2.42 3.060(5) 132.4 2_757
O3 H301 O2 0.85 2.59 3.318(4) 144.2 2_757
O3 H302 N3 0.85 2.07 2.912(4) 169.6 1_656
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max 0.553
_refine_diff_density_min -0.872
_refine_diff_density_rms 0.137
data_lq104
_database_code_depnum_ccdc_archive 'CCDC 918642'
#TrackingRef 'LQ104.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C18 H12 N6 O3 Sr, 0.5(C12 H4 N4)'
_chemical_formula_sum 'C24 H14 N8 O3 Sr'
_chemical_formula_weight 550.05
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'
Sr Sr -1.5307 3.2498 '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 9.781(2)
_cell_length_b 11.007(2)
_cell_length_c 11.382(2)
_cell_angle_alpha 80.46(3)
_cell_angle_beta 82.42(3)
_cell_angle_gamma 81.98(3)
_cell_volume 1189.2(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 9783
_cell_measurement_theta_min 3.00
_cell_measurement_theta_max 27.50
_exptl_crystal_description block
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.536
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 552
_exptl_absorpt_coefficient_mu 2.311
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6104
_exptl_absorpt_correction_T_max 0.7261
_exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 11677
_diffrn_reflns_av_R_equivalents 0.0384
_diffrn_reflns_av_sigmaI/netI 0.0532
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 3.00
_diffrn_reflns_theta_max 27.48
_reflns_number_total 5376
_reflns_number_gt 4484
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_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^)+(0.0326P)^2^+0.9429P] 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 5376
_refine_ls_number_parameters 325
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0492
_refine_ls_R_factor_gt 0.0356
_refine_ls_wR_factor_ref 0.0892
_refine_ls_wR_factor_gt 0.0755
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_restrained_S_all 1.018
_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
Sr1 Sr 0.92863(3) 0.33728(2) 0.99727(2) 0.02795(8) Uani 1 1 d . . .
C1 C 0.5796(3) 0.3931(3) 0.8582(2) 0.0342(6) Uani 1 1 d . . .
C2 C 0.4613(3) 0.3965(3) 0.7970(2) 0.0311(6) Uani 1 1 d . . .
C3 C 0.3292(3) 0.4161(3) 0.8629(3) 0.0384(7) Uani 1 1 d . . .
C4 C 0.4753(3) 0.3722(2) 0.6773(2) 0.0281(5) Uani 1 1 d . . .
C5 C 0.3561(3) 0.3639(3) 0.6196(2) 0.0335(6) Uani 1 1 d . . .
H5 H 0.2681 0.3745 0.6616 0.040 Uiso 1 1 calc R . .
C6 C 0.3689(3) 0.3410(3) 0.5053(3) 0.0322(6) Uani 1 1 d . . .
H6 H 0.2894 0.3359 0.4705 0.039 Uiso 1 1 calc R . .
C7 C 0.5007(3) 0.3245(2) 0.4372(2) 0.0282(5) Uani 1 1 d . . .
C8 C 0.6190(3) 0.3321(3) 0.4956(3) 0.0369(7) Uani 1 1 d . . .
H8 H 0.7071 0.3216 0.4538 0.044 Uiso 1 1 calc R . .
C9 C 0.6065(3) 0.3541(3) 0.6099(3) 0.0349(6) Uani 1 1 d . . .
H9 H 0.6862 0.3574 0.6451 0.042 Uiso 1 1 calc R . .
C10 C 0.5162(3) 0.3012(3) 0.3172(2) 0.0314(6) Uani 1 1 d . . .
C11 C 0.4003(3) 0.2924(3) 0.2588(3) 0.0371(6) Uani 1 1 d . . .
C12 C 0.6483(3) 0.2872(3) 0.2498(3) 0.0350(6) Uani 1 1 d . . .
C13 C 0.9802(3) 0.3469(2) 0.4643(2) 0.0321(6) Uani 1 1 d . . .
C14 C 0.9887(3) 0.2428(2) 0.5561(2) 0.0282(5) Uani 1 1 d . . .
C15 C 0.9876(3) 0.2690(2) 0.6742(2) 0.0298(6) Uani 1 1 d . . .
C16 C 0.9946(3) 0.1013(2) 0.4088(2) 0.0292(6) Uani 1 1 d . . .
H16 H 0.9914 0.1689 0.3477 0.035 Uiso 1 1 calc R . .
C17 C 0.9946(2) 0.1218(2) 0.5285(2) 0.0253(5) Uani 1 1 d . . .
C18 C 1.0010(3) 0.0160(2) 0.6188(2) 0.0299(6) Uani 1 1 d . . .
H18 H 1.0021 0.0265 0.6981 0.036 Uiso 1 1 calc R . .
C19 C 0.6079(4) 0.0663(3) 0.7853(3) 0.0497(8) Uani 1 1 d . . .
C20 C 0.4870(3) 0.0546(3) 0.7348(3) 0.0420(7) Uani 1 1 d . . .
C21 C 0.3601(4) 0.0720(3) 0.8081(3) 0.0506(8) Uani 1 1 d . . .
C22 C 0.6227(3) 0.0084(3) 0.5458(3) 0.0420(7) Uani 1 1 d . . .
H22 H 0.7048 0.0138 0.5765 0.050 Uiso 1 1 calc R . .
C23 C 0.4945(3) 0.0269(3) 0.6181(3) 0.0360(6) Uani 1 1 d . . .
C24 C 0.3717(3) 0.0169(3) 0.5668(3) 0.0432(7) Uani 1 1 d . . .
H24 H 0.2858 0.0280 0.6121 0.052 Uiso 1 1 calc R . .
N1 N 0.6769(3) 0.3912(3) 0.9051(2) 0.0465(7) Uani 1 1 d . . .
N2 N 0.2206(3) 0.4341(3) 0.9126(2) 0.0589(8) Uani 1 1 d . . .
N3 N 0.3046(3) 0.2859(3) 0.2133(3) 0.0562(8) Uani 1 1 d . . .
N4 N 0.7555(3) 0.2781(3) 0.1962(2) 0.0506(7) Uani 1 1 d . . .
N5 N 0.9860(3) 0.2923(2) 0.7687(2) 0.0415(6) Uani 1 1 d . . .
N6 N 0.9720(3) 0.4264(2) 0.3865(2) 0.0493(7) Uani 1 1 d . . .
N7 N 0.7065(4) 0.0783(3) 0.8241(3) 0.0751(11) Uani 1 1 d . . .
N8 N 0.2570(4) 0.0849(4) 0.8660(3) 0.0806(11) Uani 1 1 d . . .
O1 O 0.94559(18) 0.55238(16) 0.86221(16) 0.0304(4) Uani 1 1 d . . .
H101 H 0.9938 0.5496 0.7959 0.046 Uiso 1 1 d R . .
H102 H 0.8654 0.5893 0.8503 0.046 Uiso 1 1 d R . .
O2 O 0.8834(2) 0.12114(19) 0.9829(2) 0.0487(6) Uani 1 1 d . . .
H201 H 0.8143 0.1224 0.9464 0.073 Uiso 1 1 d R . .
H202 H 0.8838 0.0617 1.0383 0.073 Uiso 1 1 d R . .
O3 O 1.1136(2) 0.1811(2) 1.0902(2) 0.0583(7) Uani 1 1 d . . .
H301 H 1.1551 0.1166 1.0625 0.088 Uiso 1 1 d R . .
H302 H 1.1737 0.2175 1.1121 0.088 Uiso 1 1 d 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
Sr1 0.03695(14) 0.03088(13) 0.01843(13) -0.00483(9) -0.00687(9) -0.00750(10)
C1 0.0392(15) 0.0405(15) 0.0243(14) -0.0129(11) -0.0058(11) 0.0019(13)
C2 0.0302(13) 0.0368(14) 0.0276(15) -0.0105(11) -0.0061(11) 0.0016(12)
C3 0.0401(16) 0.0505(17) 0.0238(15) -0.0130(12) -0.0072(12) 0.0095(14)
C4 0.0279(12) 0.0300(13) 0.0278(14) -0.0096(10) -0.0048(10) 0.0003(11)
C5 0.0237(12) 0.0493(16) 0.0277(15) -0.0114(12) -0.0033(10) 0.0019(12)
C6 0.0224(12) 0.0440(15) 0.0324(15) -0.0119(12) -0.0067(10) -0.0002(12)
C7 0.0270(12) 0.0324(13) 0.0267(14) -0.0100(11) -0.0050(10) -0.0005(11)
C8 0.0233(12) 0.0590(19) 0.0320(16) -0.0175(13) -0.0011(11) -0.0065(13)
C9 0.0241(12) 0.0520(17) 0.0333(16) -0.0180(13) -0.0055(11) -0.0047(12)
C10 0.0294(13) 0.0407(15) 0.0267(14) -0.0125(11) -0.0063(11) -0.0013(12)
C11 0.0403(15) 0.0457(16) 0.0278(15) -0.0106(12) -0.0090(12) -0.0023(13)
C12 0.0383(15) 0.0440(16) 0.0246(15) -0.0115(12) -0.0060(12) -0.0019(13)
C13 0.0380(14) 0.0332(14) 0.0271(15) -0.0106(11) 0.0001(11) -0.0070(12)
C14 0.0307(13) 0.0330(13) 0.0212(13) -0.0077(10) -0.0019(10) -0.0021(11)
C15 0.0354(14) 0.0271(13) 0.0269(15) -0.0047(10) -0.0013(11) -0.0048(11)
C16 0.0347(13) 0.0323(13) 0.0202(13) -0.0024(10) -0.0039(10) -0.0044(11)
C17 0.0232(11) 0.0307(12) 0.0228(13) -0.0077(10) -0.0008(9) -0.0029(10)
C18 0.0344(13) 0.0389(14) 0.0175(13) -0.0058(10) -0.0046(10) -0.0052(12)
C19 0.064(2) 0.0470(18) 0.043(2) -0.0145(15) -0.0224(17) 0.0001(17)
C20 0.0465(17) 0.0391(16) 0.0432(19) -0.0105(13) -0.0117(14) -0.0034(14)
C21 0.066(2) 0.0479(19) 0.038(2) -0.0057(15) -0.0036(17) -0.0093(17)
C22 0.0267(13) 0.0519(18) 0.053(2) -0.0204(15) -0.0142(13) -0.0012(13)
C23 0.0333(14) 0.0345(14) 0.0436(18) -0.0126(12) -0.0109(12) -0.0009(12)
C24 0.0277(14) 0.0548(18) 0.051(2) -0.0180(15) -0.0094(13) -0.0028(14)
N1 0.0421(14) 0.0631(17) 0.0376(15) -0.0188(13) -0.0129(12) 0.0032(13)
N2 0.0427(15) 0.098(2) 0.0291(15) -0.0132(15) -0.0020(12) 0.0183(16)
N3 0.0478(16) 0.075(2) 0.0510(19) -0.0195(15) -0.0218(14) 0.0005(15)
N4 0.0447(15) 0.074(2) 0.0314(15) -0.0127(13) 0.0030(12) -0.0016(14)
N5 0.0641(17) 0.0367(13) 0.0244(13) -0.0091(10) -0.0010(11) -0.0067(12)
N6 0.077(2) 0.0400(14) 0.0301(15) -0.0032(12) -0.0030(13) -0.0105(14)
N7 0.078(2) 0.085(2) 0.074(3) -0.033(2) -0.043(2) 0.0058(19)
N8 0.080(2) 0.097(3) 0.056(2) -0.004(2) 0.0168(19) -0.015(2)
O1 0.0315(9) 0.0370(10) 0.0221(10) -0.0076(8) -0.0019(7) 0.0011(8)
O2 0.0665(14) 0.0422(12) 0.0439(14) -0.0005(10) -0.0217(11) -0.0211(11)
O3 0.0495(13) 0.0442(12) 0.090(2) -0.0281(13) -0.0315(13) 0.0085(11)
_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
Sr1 O2 2.515(2) . ?
Sr1 O3 2.526(2) . ?
Sr1 O1 2.614(2) . ?
Sr1 O1 2.6695(19) 2_767 ?
Sr1 N4 2.688(3) 1_556 ?
Sr1 N5 2.700(3) . ?
Sr1 N1 2.754(3) . ?
Sr1 N2 2.991(3) 2_667 ?
Sr1 N2 3.163(3) 1_655 ?
Sr1 H201 2.9224 . ?
Sr1 H302 2.9270 . ?
C1 N1 1.148(4) . ?
C1 C2 1.420(4) . ?
C2 C3 1.414(4) . ?
C2 C4 1.417(4) . ?
C3 N2 1.144(4) . ?
C4 C9 1.413(4) . ?
C4 C5 1.432(3) . ?
C5 C6 1.352(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.419(4) . ?
C6 H6 0.9300 . ?
C7 C10 1.417(4) . ?
C7 C8 1.426(4) . ?
C8 C9 1.349(4) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.409(4) . ?
C10 C12 1.415(4) . ?
C11 N3 1.144(4) . ?
C12 N4 1.142(4) . ?
C13 N6 1.139(4) . ?
C13 C14 1.418(4) . ?
C14 C17 1.411(4) . ?
C14 C15 1.419(4) . ?
C15 N5 1.144(4) . ?
C16 C18 1.373(4) 2_756 ?
C16 C17 1.418(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.419(4) . ?
C18 C16 1.373(4) 2_756 ?
C18 H18 0.9300 . ?
C19 N7 1.144(4) . ?
C19 C20 1.411(4) . ?
C20 C23 1.402(4) . ?
C20 C21 1.409(5) . ?
C21 N8 1.134(5) . ?
C22 C24 1.348(4) 2_656 ?
C22 C23 1.416(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.428(4) . ?
C24 C22 1.348(4) 2_656 ?
C24 H24 0.9300 . ?
N2 Sr1 2.991(3) 2_667 ?
N2 Sr1 3.163(3) 1_455 ?
N4 Sr1 2.688(3) 1_554 ?
O1 Sr1 2.6695(19) 2_767 ?
O1 H101 0.8387 . ?
O1 H102 0.8486 . ?
O2 H201 0.8364 . ?
O2 H202 0.8302 . ?
O3 H301 0.8531 . ?
O3 H302 0.8397 . ?
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
O2 Sr1 O3 70.21(7) . . ?
O2 Sr1 O1 139.90(7) . . ?
O3 Sr1 O1 130.95(7) . . ?
O2 Sr1 O1 137.65(6) . 2_767 ?
O3 Sr1 O1 71.39(7) . 2_767 ?
O1 Sr1 O1 80.44(6) . 2_767 ?
O2 Sr1 N4 76.67(9) . 1_556 ?
O3 Sr1 N4 88.01(9) . 1_556 ?
O1 Sr1 N4 129.09(8) . 1_556 ?
O1 Sr1 N4 84.87(8) 2_767 1_556 ?
O2 Sr1 N5 69.50(8) . . ?
O3 Sr1 N5 98.70(9) . . ?
O1 Sr1 N5 73.30(7) . . ?
O1 Sr1 N5 134.13(7) 2_767 . ?
N4 Sr1 N5 140.60(9) 1_556 . ?
O2 Sr1 N1 80.52(8) . . ?
O3 Sr1 N1 150.19(8) . . ?
O1 Sr1 N1 76.15(8) . . ?
O1 Sr1 N1 133.34(7) 2_767 . ?
N4 Sr1 N1 79.67(9) 1_556 . ?
N5 Sr1 N1 75.47(8) . . ?
O2 Sr1 N2 139.04(9) . 2_667 ?
O3 Sr1 N2 128.50(8) . 2_667 ?
O1 Sr1 N2 60.97(7) . 2_667 ?
O1 Sr1 N2 61.44(7) 2_767 2_667 ?
N4 Sr1 N2 69.15(9) 1_556 2_667 ?
N5 Sr1 N2 128.50(8) . 2_667 ?
N1 Sr1 N2 71.91(8) . 2_667 ?
O2 Sr1 N2 122.81(8) . 1_655 ?
O3 Sr1 N2 71.55(8) . 1_655 ?
O1 Sr1 N2 59.48(7) . 1_655 ?
O1 Sr1 N2 58.05(7) 2_767 1_655 ?
N4 Sr1 N2 141.48(8) 1_556 1_655 ?
N5 Sr1 N2 76.20(8) . 1_655 ?
N1 Sr1 N2 132.46(8) . 1_655 ?
N2 Sr1 N2 98.12(7) 2_667 1_655 ?
O2 Sr1 Sr1 169.93(6) . 2_767 ?
O3 Sr1 Sr1 102.32(6) . 2_767 ?
O1 Sr1 Sr1 40.73(4) . 2_767 ?
O1 Sr1 Sr1 39.71(4) 2_767 2_767 ?
N4 Sr1 Sr1 110.45(7) 1_556 2_767 ?
N5 Sr1 Sr1 105.94(6) . 2_767 ?
N1 Sr1 Sr1 107.40(7) . 2_767 ?
N2 Sr1 Sr1 50.90(7) 2_667 2_767 ?
N2 Sr1 Sr1 47.22(6) 1_655 2_767 ?
O2 Sr1 H201 15.5 . . ?
O3 Sr1 H201 85.7 . . ?
O1 Sr1 H201 128.3 . . ?
O1 Sr1 H201 151.3 2_767 . ?
N4 Sr1 H201 77.1 1_556 . ?
N5 Sr1 H201 64.9 . . ?
N1 Sr1 H201 65.2 . . ?
N2 Sr1 H201 129.0 2_667 . ?
N2 Sr1 H201 131.0 1_655 . ?
Sr1 Sr1 H201 169.0 2_767 . ?
O2 Sr1 H302 85.8 . . ?
O3 Sr1 H302 15.6 . . ?
O1 Sr1 H302 117.9 . . ?
O1 Sr1 H302 57.1 2_767 . ?
N4 Sr1 H302 92.6 1_556 . ?
N5 Sr1 H302 104.2 . . ?
N1 Sr1 H302 165.5 . . ?
N2 Sr1 H302 117.0 2_667 . ?
N2 Sr1 H302 59.9 1_655 . ?
Sr1 Sr1 H302 86.8 2_767 . ?
H201 Sr1 H302 101.2 . . ?
N1 C1 C2 178.4(3) . . ?
C3 C2 C4 121.3(2) . . ?
C3 C2 C1 117.3(2) . . ?
C4 C2 C1 121.2(2) . . ?
N2 C3 C2 177.6(3) . . ?
C9 C4 C2 121.9(2) . . ?
C9 C4 C5 117.0(2) . . ?
C2 C4 C5 121.1(2) . . ?
C6 C5 C4 121.3(2) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 121.5(2) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C10 C7 C6 122.4(2) . . ?
C10 C7 C8 120.9(2) . . ?
C6 C7 C8 116.8(2) . . ?
C9 C8 C7 121.8(2) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C4 121.6(2) . . ?
C8 C9 H9 119.2 . . ?
C4 C9 H9 119.2 . . ?
C11 C10 C12 116.9(3) . . ?
C11 C10 C7 121.4(2) . . ?
C12 C10 C7 121.7(2) . . ?
N3 C11 C10 178.7(3) . . ?
N4 C12 C10 178.5(3) . . ?
N6 C13 C14 176.4(3) . . ?
C17 C14 C13 120.4(2) . . ?
C17 C14 C15 123.5(2) . . ?
C13 C14 C15 116.1(2) . . ?
N5 C15 C14 178.8(3) . . ?
C18 C16 C17 121.4(2) 2_756 . ?
C18 C16 H16 119.3 2_756 . ?
C17 C16 H16 119.3 . . ?
C14 C17 C16 120.9(2) . . ?
C14 C17 C18 121.6(2) . . ?
C16 C17 C18 117.4(2) . . ?
C16 C18 C17 121.2(2) 2_756 . ?
C16 C18 H18 119.4 2_756 . ?
C17 C18 H18 119.4 . . ?
N7 C19 C20 178.3(4) . . ?
C23 C20 C21 122.5(3) . . ?
C23 C20 C19 121.2(3) . . ?
C21 C20 C19 116.3(3) . . ?
N8 C21 C20 178.8(4) . . ?
C24 C22 C23 121.4(3) 2_656 . ?
C24 C22 H22 119.3 2_656 . ?
C23 C22 H22 119.3 . . ?
C20 C23 C22 122.0(3) . . ?
C20 C23 C24 121.0(3) . . ?
C22 C23 C24 117.0(3) . . ?
C22 C24 C23 121.6(3) 2_656 . ?
C22 C24 H24 119.2 2_656 . ?
C23 C24 H24 119.2 . . ?
C1 N1 Sr1 167.1(2) . . ?
C3 N2 Sr1 130.7(3) . 2_667 ?
C3 N2 Sr1 146.9(3) . 1_455 ?
Sr1 N2 Sr1 81.88(7) 2_667 1_455 ?
C12 N4 Sr1 151.0(2) . 1_554 ?
C15 N5 Sr1 168.4(2) . . ?
Sr1 O1 Sr1 99.56(6) . 2_767 ?
Sr1 O1 H101 114.8 . . ?
Sr1 O1 H101 110.2 2_767 . ?
Sr1 O1 H102 110.9 . . ?
Sr1 O1 H102 112.3 2_767 . ?
H101 O1 H102 108.9 . . ?
Sr1 O2 H201 111.1 . . ?
Sr1 O2 H202 125.9 . . ?
H201 O2 H202 108.6 . . ?
Sr1 O3 H301 126.8 . . ?
Sr1 O3 H302 110.4 . . ?
H301 O3 H302 108.0 . . ?
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
O1 H101 N6 0.84 2.04 2.820(3) 155.0 2_766
O1 H102 N3 0.85 2.13 2.955(3) 164.8 2_666
O2 H201 N7 0.84 2.01 2.797(4) 156.3 .
O2 H202 N8 0.83 2.31 2.990(4) 139.7 2_657
O3 H301 N7 0.85 2.61 3.213(4) 128.3 2_757
O3 H301 O2 0.85 2.83 3.556(3) 143.5 2_757
O3 H302 N3 0.84 2.12 2.934(4) 164.6 1_656
_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full 27.48
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max 0.339
_refine_diff_density_min -0.488
_refine_diff_density_rms 0.075