#------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100124.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100124
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H22 N9 O11 Pr'
_chemical_formula_weight         777.44
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           ?
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.61
_cell_angle_beta                 96.13
_cell_angle_gamma                103.19
_cell_formula_units_Z            2
_cell_length_a                   7.780
_cell_length_b                   11.326
_cell_length_c                   17.873
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     1523.6
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    ?
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6556
_diffrn_reflns_theta_full        21.02
_diffrn_reflns_theta_max         21.02
_diffrn_reflns_theta_min         1.15
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             776
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_refine_diff_density_max         0.610
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0352P)²+1.9831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                3135
_reflns_number_total             3279
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               1100124
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr Pr 0.37530(3) 0.279253(18) 0.736020(12) 0.02953(13) Uani 1 1 d . . .
O2 O 0.7956(5) 0.1159(4) 0.8139(3) 0.0822(13) Uani 1 1 d . . .
O5 O 0.3632(4) 0.4830(3) 0.79011(17) 0.0426(8) Uani 1 1 d . . .
O6 O 0.4003(5) 0.2442(3) 0.60103(17) 0.0493(8) Uani 1 1 d . . .
O7 O 0.6428(5) 0.4364(3) 0.6951(2) 0.0539(9) Uani 1 1 d . . .
O8 O 0.5364(5) 0.1463(3) 0.8267(2) 0.0618(10) Uani 1 1 d . . .
O9 O 0.6433(5) 0.1817(3) 0.7226(2) 0.0561(9) Uani 1 1 d . . .
N10 N 0.3023(5) 0.2995(3) 0.8823(2) 0.0414(9) Uani 1 1 d . . .
O11 O 0.6836(5) 0.3943(3) 0.81102(19) 0.0523(8) Uani 1 1 d . . .
O12 O 0.3040(5) 0.4179(3) 0.9064(2) 0.0627(10) Uani 1 1 d . . .
O13 O 0.1698(5) 0.0803(3) 0.7835(2) 0.0560(9) Uani 1 1 d . . .
O21 O 0.2197(9) 0.0718(4) 0.6716(3) 0.128(2) Uani 1 1 d . . .
O22 O 0.9032(5) 0.4925(3) 0.7549(2) 0.0712(11) Uani 1 1 d . . .
O32 O 0.0730(6) -0.0863(3) 0.7200(2) 0.0823(13) Uani 1 1 d . . .
N14 N 0.7478(5) 0.4434(3) 0.7495(3) 0.0373(9) Uani 1 1 d . . .
N16 N 0.6611(6) 0.1464(3) 0.7888(3) 0.0496(11) Uani 1 1 d . . .
N17 N 0.3048(5) 0.3995(4) 0.5523(2) 0.0363(9) Uani 1 1 d . . .
H14 H 0.278(5) 0.438(4) 0.519(3) 0.027(13) Uiso 1 1 d . . .
N18 N 0.3376(6) 0.5040(4) 0.8550(3) 0.0566(11) Uani 1 1 d . . .
C19 C 0.3434(6) 0.6310(4) 0.8847(2) 0.0373(11) Uani 1 1 d . . .
O20 O 0.0566(6) 0.2839(5) 0.7301(3) 0.0602(12) Uani 1 1 d . . .
H20A H 0.035(10) 0.328(6) 0.741(4) 0.07(3) Uiso 1 1 d . . .
H20B H -0.020(11) 0.236(7) 0.754(4) 0.11(3) Uiso 1 1 d . . .
N25 N 0.1537(5) 0.0205(3) 0.7245(2) 0.0390(9) Uani 1 1 d . . .
N30 N 0.2816(5) 0.4380(3) 0.6236(2) 0.0403(9) Uani 1 1 d . . .
N15 N 0.2034(5) 0.5951(3) 0.4989(2) 0.0417(9) Uani 1 1 d . . .
N23 N 0.1892(5) 0.3371(3) 1.0308(2) 0.0458(10) Uani 1 1 d . . .
C24 C 0.2589(7) 0.2179(5) 0.9299(3) 0.0447(12) Uani 1 1 d . . .
H13 H 0.263(7) 0.143(5) 0.914(3) 0.062(16) Uiso 1 1 d . . .
C27 C 0.3863(8) 0.0824(5) 0.3892(3) 0.0627(15) Uani 1 1 d . . .
H13 H 0.399(8) 0.003(6) 0.380(3) 0.078(18) Uiso 1 1 d . . .
C28 C 0.2027(6) 0.2275(4) 1.0043(2) 0.0396(11) Uani 1 1 d . . .
C29 C 0.3787(7) 0.7234(4) 0.8350(3) 0.0492(12) Uani 1 1 d . . .
H29 H 0.394(6) 0.707(4) 0.784(3) 0.045(13) Uiso 1 1 d . . .
C31 C 0.1890(6) 0.6201(4) 0.5724(3) 0.0401(11) Uani 1 1 d . . .
C34 C 0.3436(6) 0.3152(5) 0.4051(3) 0.0427(12) Uani 1 1 d . . .
H12 H 0.325(6) 0.391(5) 0.408(3) 0.051(14) Uiso 1 1 d . . .
C35 C 0.1324(7) 0.3424(5) 1.0981(3) 0.0510(13) Uani 1 1 d . . .
H18 H 0.118(8) 0.414(6) 1.111(3) 0.08(2) Uiso 1 1 d . . .
C36 C 0.3640(6) 0.2503(4) 0.4677(2) 0.0360(11) Uani 1 1 d . . .
C37 C 0.1076(8) 0.8047(5) 0.5421(4) 0.0601(15) Uani 1 1 d . . .
H4 H 0.082(8) 0.879(6) 0.566(4) 0.09(2) Uiso 1 1 d . . .
C38 C 0.1399(7) 0.7246(5) 0.5947(3) 0.0490(13) Uani 1 1 d . . .
H25 H 0.137(7) 0.737(5) 0.645(3) 0.063(16) Uiso 1 1 d . . .
C42 C 0.3593(6) 0.2976(4) 0.5456(3) 0.0394(11) Uani 1 1 d . . .
C43 C 0.1619(7) 0.1249(5) 1.0469(3) 0.0462(12) Uani 1 1 d . . .
H15 H 0.170(6) 0.054(5) 1.028(3) 0.051(14) Uiso 1 1 d . . .
C44 C 0.1697(6) 0.6763(5) 0.4494(3) 0.0453(12) Uani 1 1 d . . .
H18 H 0.187(6) 0.663(4) 0.401(3) 0.042(13) Uiso 1 1 d . . .
C45 C 0.1218(7) 0.7809(5) 0.4690(4) 0.0560(14) Uani 1 1 d . . .
H9 H 0.095(6) 0.829(5) 0.433(3) 0.048(14) Uiso 1 1 d . . .
C46 C 0.3631(8) 0.8672(5) 0.9305(4) 0.0638(17) Uani 1 1 d . . .
H2 H 0.375(10) 0.944(7) 0.951(4) 0.11(2) Uiso 1 1 d . . .
C47 C 0.3447(7) 0.2654(5) 0.3353(3) 0.0512(13) Uani 1 1 d . . .
H10 H 0.332(6) 0.310(5) 0.293(3) 0.053(14) Uiso 1 1 d . . .
C48 C 0.1057(7) 0.1352(6) 1.1161(3) 0.0525(15) Uani 1 1 d . . .
H8 H 0.074(6) 0.077(5) 1.140(3) 0.044(15) Uiso 1 1 d . . .
C49 C 0.3871(8) 0.8406(5) 0.8590(4) 0.0619(15) Uani 1 1 d . . .
H12 H 0.423(8) 0.898(6) 0.828(4) 0.08(2) Uiso 1 1 d . . .
C50 C 0.0897(7) 0.2453(5) 1.1414(3) 0.0492(13) Uani 1 1 d . . .
H24 H 0.055(7) 0.252(5) 1.185(4) 0.063(17) Uiso 1 1 d . . .
C51 C 0.3860(8) 0.1342(5) 0.4598(3) 0.0532(14) Uani 1 1 d . . .
H7 H 0.396(7) 0.097(5) 0.496(3) 0.054(17) Uiso 1 1 d . . .
C52 C 0.3272(8) 0.7753(6) 0.9804(4) 0.0638(17) Uani 1 1 d . . .
H21 H 0.320(8) 0.788(6) 1.025(4) 0.07(2) Uiso 1 1 d . . .
C54 C 0.3172(7) 0.6564(5) 0.9572(3) 0.0484(13) Uani 1 1 d . . .
H19 H 0.296(6) 0.602(4) 0.991(3) 0.045(15) Uiso 1 1 d . . .
C55 C 0.2281(6) 0.5357(4) 0.6298(3) 0.0424(11) Uani 1 1 d . . .
H5 H 0.216(6) 0.559(4) 0.683(3) 0.045(12) Uiso 1 1 d . . .
C56 C 0.3630(8) 0.1487(5) 0.3265(3) 0.0561(14) Uani 1 1 d . . .
H10 H 0.361(7) 0.111(5) 0.275(3) 0.072(16) Uiso 1 1 d . . .
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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Pr O20 100.42(15) . . ?
O6 Pr O5 122.60(10) . . ?
O20 Pr O5 73.09(16) . . ?
O6 Pr O21 60.81(13) . . ?
O20 Pr O21 77.7(2) . . ?
O5 Pr O21 150.73(19) . . ?
O6 Pr O7 70.23(12) . . ?
O20 Pr O7 130.52(15) . . ?
O5 Pr O7 72.84(10) . . ?
O21 Pr O7 127.74(13) . . ?
O6 Pr O9 70.29(11) . . ?
O20 Pr O9 155.77(16) . . ?
O5 Pr O9 130.99(11) . . ?
O21 Pr O9 78.28(18) . . ?
O7 Pr O9 68.77(11) . . ?
O6 Pr O8 113.76(12) . . ?
O20 Pr O8 125.34(14) . . ?
O5 Pr O8 115.51(11) . . ?
O21 Pr O8 83.26(18) . . ?
O7 Pr O8 101.47(12) . . ?
O9 Pr O8 47.81(11) . . ?
O6 Pr O13 107.63(11) . . ?
O20 Pr O13 65.77(15) . . ?
O5 Pr O13 119.22(11) . . ?
O21 Pr O13 46.85(12) . . ?
O7 Pr O13 163.59(12) . . ?
O9 Pr O13 95.02(12) . . ?
O8 Pr O13 63.91(11) . . ?
O6 Pr O11 112.24(11) . . ?
O20 Pr O11 138.15(16) . . ?
O5 Pr O11 67.56(10) . . ?
O21 Pr O11 141.04(19) . . ?
O7 Pr O11 48.03(11) . . ?
O9 Pr O11 64.30(10) . . ?
O8 Pr O11 64.05(11) . . ?
O13 Pr O11 123.43(11) . . ?
O6 Pr N10 172.37(11) . . ?
O20 Pr N10 73.27(14) . . ?
O5 Pr N10 60.31(10) . . ?
O21 Pr N10 112.91(13) . . ?
O7 Pr N10 117.06(11) . . ?
O9 Pr N10 113.72(11) . . ?
O8 Pr N10 68.11(11) . . ?
O13 Pr N10 66.10(11) . . ?
O11 Pr N10 75.33(11) . . ?
O6 Pr N30 58.11(10) . . ?
O20 Pr N30 68.48(13) . . ?
O5 Pr N30 67.23(10) . . ?
O21 Pr N30 100.16(16) . . ?
O7 Pr N30 65.74(11) . . ?
O9 Pr N30 119.41(11) . . ?
O8 Pr N30 166.14(11) . . ?
O13 Pr N30 127.84(11) . . ?
O11 Pr N30 107.16(10) . . ?
N10 Pr N30 121.59(10) . . ?
N18 O5 Pr 125.6(3) . . ?
C42 O6 Pr 131.1(3) . . ?
N14 O7 Pr 101.0(3) . . ?
N16 O8 Pr 96.4(3) . . ?
N16 O9 Pr 97.5(3) . . ?
C24 N10 O12 115.4(4) . . ?
C24 N10 Pr 130.3(3) . . ?
O12 N10 Pr 114.2(2) . . ?
N14 O11 Pr 93.4(2) . . ?
N18 O12 N10 116.1(4) . . ?
N25 O13 Pr 95.9(2) . . ?
N25 O21 Pr 99.9(3) . . ?
O7 N14 O22 126.9(5) . . ?
O7 N14 O11 115.8(4) . . ?
O22 N14 O11 117.2(4) . . ?
O2 N16 O8 122.6(5) . . ?
O2 N16 O9 121.0(5) . . ?
O8 N16 O9 116.4(4) . . ?
C42 N17 N30 118.2(4) . . ?
O5 N18 O12 123.6(4) . . ?
O5 N18 C19 122.4(4) . . ?
O12 N18 C19 113.9(4) . . ?
C54 C19 C29 120.0(4) . . ?
C54 C19 N18 123.3(4) . . ?
C29 C19 N18 116.7(4) . . ?
O21 N25 O13 117.1(4) . . ?
O21 N25 O32 122.2(4) . . ?
O13 N25 O32 120.6(4) . . ?
C55 N30 N17 118.1(4) . . ?
C55 N30 Pr 130.4(3) . . ?
N17 N30 Pr 111.5(3) . . ?
C44 N15 C31 116.7(4) . . ?
C35 N23 C28 117.7(4) . . ?
N10 C24 C28 130.1(4) . . ?
C56 C27 C51 119.2(5) . . ?
N23 C28 C43 120.9(4) . . ?
N23 C28 C24 119.1(4) . . ?
C43 C28 C24 120.1(4) . . ?
C49 C29 C19 119.4(6) . . ?
N15 C31 C38 121.7(4) . . ?
N15 C31 C55 119.3(4) . . ?
C38 C31 C55 119.0(4) . . ?
C36 C34 C47 120.5(5) . . ?
N23 C35 C50 123.8(5) . . ?
C34 C36 C51 119.1(4) . . ?
C34 C36 C42 123.4(4) . . ?
C51 C36 C42 117.5(4) . . ?
C45 C37 C38 119.5(5) . . ?
C37 C38 C31 119.2(5) . . ?
O6 C42 N17 120.8(4) . . ?
O6 C42 C36 121.8(4) . . ?
N17 C42 C36 117.3(4) . . ?
C48 C43 C28 119.2(5) . . ?
N15 C44 C45 123.4(5) . . ?
C37 C45 C44 119.3(5) . . ?
C49 C46 C52 119.6(5) . . ?
C34 C47 C56 121.0(5) . . ?
C50 C48 C43 119.2(5) . . ?
C46 C49 C29 121.3(6) . . ?
C35 C50 C48 119.2(5) . . ?
C36 C51 C27 120.9(5) . . ?
C46 C52 C54 119.9(6) . . ?
C19 C54 C52 119.8(6) . . ?
N30 C55 C31 130.3(4) . . ?
C27 C56 C47 119.3(5) . . ?
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
Pr O6 2.476(3) . ?
Pr O20 2.484(4) . ?
Pr O5 2.518(3) . ?
Pr O21 2.580(4) . ?
Pr O7 2.588(3) . ?
Pr O9 2.603(3) . ?
Pr O8 2.635(3) . ?
Pr O13 2.653(3) . ?
Pr O11 2.664(3) . ?
Pr N10 2.753(4) . ?
Pr N30 2.858(4) . ?
O2 N16 1.218(5) . ?
O5 N18 1.227(5) . ?
O6 C42 1.218(5) . ?
O7 N14 1.192(5) . ?
O8 N16 1.240(5) . ?
O9 N16 1.257(5) . ?
N10 C24 1.276(6) . ?
N10 O12 1.400(5) . ?
O11 N14 1.331(5) . ?
O12 N18 1.349(6) . ?
O13 N25 1.225(5) . ?
O21 N25 1.214(6) . ?
O22 N14 1.203(5) . ?
O32 N25 1.227(5) . ?
N17 C42 1.325(6) . ?
N17 N30 1.385(5) . ?
N18 C19 1.517(6) . ?
C19 C54 1.370(7) . ?
C19 C29 1.378(7) . ?
N30 C55 1.275(6) . ?
N15 C44 1.333(6) . ?
N15 C31 1.363(6) . ?
N23 C35 1.330(6) . ?
N23 C28 1.354(6) . ?
C24 C28 1.454(7) . ?
C27 C56 1.374(8) . ?
C27 C51 1.387(8) . ?
C28 C43 1.390(7) . ?
C29 C49 1.376(8) . ?
C31 C38 1.391(7) . ?
C31 C55 1.464(7) . ?
C34 C36 1.361(7) . ?
C34 C47 1.365(7) . ?
C35 C50 1.351(8) . ?
C36 C51 1.372(7) . ?
C36 C42 1.493(6) . ?
C37 C45 1.352(8) . ?
C37 C38 1.357(8) . ?
C43 C48 1.368(7) . ?
C44 C45 1.373(7) . ?
C46 C49 1.352(9) . ?
C46 C52 1.378(9) . ?
C47 C56 1.371(7) . ?
C48 C50 1.359(8) . ?
C52 C54 1.387(8) . ?
