# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_CP_1
_database_code_depnum_ccdc_archive 'CCDC 1838574'
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-10-02 downloaded from the CCDC.
;
_audit_creation_date 2018-01-23
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H32 Gd4 O34 S4, 4.6(H2 O), 1.4(C2 H3 N1)'
_chemical_formula_sum 'C30.80 H45.40 Gd4 N1.40 O38.60 S4'
_chemical_formula_weight 1810.12
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Gd Gd -0.1653 3.9035 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system tetragonal
_space_group_IT_number 82
_space_group_name_H-M_alt 'I -4'
_space_group_name_Hall 'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
_cell_length_a 12.9717(5)
_cell_length_b 12.9717(5)
_cell_length_c 16.3190(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2745.9(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9952
_cell_measurement_temperature 139(2)
_cell_measurement_theta_max 30.48
_cell_measurement_theta_min 2.50
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 5.025
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.4761
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0989 before and 0.0605 after correction. The Ratio of minimum to maximum transmission is 0.6381. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.189
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1738
_exptl_crystal_size_max 0.44
_exptl_crystal_size_mid 0.41
_exptl_crystal_size_min 0.23
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0434
_diffrn_reflns_av_unetI/netI 0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 22321
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.994
_diffrn_reflns_theta_min 2.496
_diffrn_ambient_temperature 139.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.932
_reflns_Friedel_fraction_full 0.997
_reflns_Friedel_fraction_max 0.998
_reflns_number_gt 3943
_reflns_number_total 4010
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.706
_refine_diff_density_min -0.864
_refine_diff_density_rms 0.097
_refine_ls_abs_structure_details
;
Flack x determined using 1864 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.007(5)
_refine_ls_extinction_coef 0.00176(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 220
_refine_ls_number_reflns 4010
_refine_ls_number_restraints 37
_refine_ls_R_factor_all 0.0186
_refine_ls_R_factor_gt 0.0180
_refine_ls_restrained_S_all 1.058
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+1.8825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0389
_refine_ls_wR_factor_ref 0.0391
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
O2L-H2LA = O2L-H2LB
0.85 with sigma of 0.02
O1L-H1LA = O1L-H1LB
0.85 with sigma of 0.02
C9-C1
1.456 with sigma of 0.01
N10-C1
2.593 with sigma of 0.02
H2LA-H2LB
1.34 with sigma of 0.04
H1LA-H1LB
1.34 with sigma of 0.04
Gd1-H2LA \\sim Gd1-H2LB
with sigma of 0.02
Gd1-H1LA \\sim Gd1-H1LB
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C9 \\sim N10: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
C1, C9, N10
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
N10, C1, C9
with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
Fixed Sof: C1(0.35) H1A(0.35) H1B(0.35) H1C(0.35) C9(0.35) N10(0.35)
O0AA(0.15) H0AA(0.15) H0AB(0.15)
6.a Riding coordinates:
O0AA(H0AA,H0AB)
6.b Free rotating group:
O1W(H1WA,H1WB)
6.c Aromatic/amide H refined with riding coordinates:
C7(H7), C6(H6), C3(H3)
6.d Idealised Me refined as rotating group:
C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd -0.65237(2) 0.03135(2) -0.32688(2) 0.00818(6) Uani 1 1 d D . . . .
O1 O -0.4833(2) 0.1014(2) -0.31457(16) 0.0097(5) Uani 1 1 d . . . . .
O3 O -0.6588(2) -0.2457(2) -0.24388(19) 0.0200(6) Uani 1 1 d . . . . .
O5 O -1.000000 -0.500000 -0.4271(2) 0.0137(8) Uani 1 2 d S T P . .
O2L O -0.8343(2) 0.0455(2) -0.37595(19) 0.0194(6) Uani 1 1 d D . . . .
H2LA H -0.858(3) 0.103(2) -0.384(3) 0.029 Uiso 1 1 d DR . . . .
H2LB H -0.846(3) 0.012(4) -0.420(2) 0.029 Uiso 1 1 d DR . . . .
S1 S -1.06259(7) -0.28832(7) -0.46462(6) 0.01173(18) Uani 1 1 d . . . . .
O6 O -1.0531(2) -0.1774(2) -0.47466(19) 0.0184(6) Uani 1 1 d . . . . .
O7 O -1.1579(2) -0.3183(3) -0.42347(18) 0.0195(7) Uani 1 1 d . . . . .
C4 C -0.9583(3) -0.3252(3) -0.4004(2) 0.0103(7) Uani 1 1 d . . . . .
C0AA C -0.7349(3) -0.2094(3) -0.2817(2) 0.0136(7) Uani 1 1 d . . . . .
C2AA C -0.8124(3) -0.2845(3) -0.3145(2) 0.0119(7) Uani 1 1 d . . . . .
C7 C -0.8005(3) -0.3889(3) -0.2965(2) 0.0147(7) Uani 1 1 d . . . . .
H7 H -0.748411 -0.409821 -0.261023 0.018 Uiso 1 1 calc R . . . .
C6 C -0.8654(3) -0.4616(3) -0.3307(3) 0.0154(7) Uani 1 1 d . . . . .
H6 H -0.857359 -0.531135 -0.318274 0.018 Uiso 1 1 calc R . . . .
C5 C -0.9427(3) -0.4297(3) -0.3838(2) 0.0114(7) Uani 1 1 d . . . . .
C3 C -0.8926(3) -0.2525(3) -0.3660(2) 0.0128(7) Uani 1 1 d . . . . .
H3 H -0.901917 -0.182771 -0.377042 0.015 Uiso 1 1 calc R . . . .
O2 O -0.7508(2) -0.1141(2) -0.29353(18) 0.0163(6) Uani 1 1 d . . . . .
O1L O -0.6565(3) 0.1792(3) -0.4200(2) 0.0224(7) Uani 1 1 d D . . . .
H1LA H -0.702(3) 0.223(3) -0.421(3) 0.034 Uiso 1 1 d DR . . . .
H1LB H -0.604(3) 0.201(4) -0.446(3) 0.034 Uiso 1 1 d DR . . . .
O1W O -0.4702(4) 0.2543(3) -0.4608(3) 0.0536(14) Uani 1 1 d . . . . .
H1WA H -0.428532 0.212029 -0.482867 0.080 Uiso 1 1 d G . . . .
H1WB H -0.497134 0.286309 -0.500908 0.080 Uiso 1 1 d G . . . .
O4 O -1.0504(2) -0.3445(2) -0.54211(16) 0.0128(5) Uani 1 1 d . . . . .
C1 C -0.491(3) 0.506(4) -0.2674(10) 0.060(4) Uani 0.35 1 d D U . A -1
H1A H -0.544916 0.457147 -0.255922 0.090 Uiso 0.35 1 calc GR . . A -1
H1B H -0.514626 0.574126 -0.254355 0.090 Uiso 0.35 1 calc GR . . A -1
H1C H -0.431608 0.489790 -0.234871 0.090 Uiso 0.35 1 calc GR . . A -1
C9 C -0.4642(15) 0.501(2) -0.3541(10) 0.058(4) Uani 0.35 1 d D U . A -1
N10 N -0.4143(13) 0.4483(16) -0.4081(11) 0.051(3) Uani 0.35 1 d D U . A -1
O0AA O -0.434(5) 0.499(5) -0.418(4) 0.11(2) Uiso 0.15 1 d . . . B -2
H0AA H -0.483501 0.504714 -0.384314 0.168 Uiso 0.15 1 d R . . B -2
H0AB H -0.386171 0.470024 -0.390474 0.168 Uiso 0.15 1 d R . . B -2
H1 H -0.467(4) 0.143(4) -0.339(3) 0.025(15) 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
Gd1 0.00897(9) 0.00770(9) 0.00786(8) -0.00062(6) -0.00170(6) 0.00074(7)
O1 0.0116(12) 0.0088(11) 0.0088(13) 0.0019(9) 0.0016(9) 0.0005(11)
O3 0.0196(15) 0.0196(15) 0.0208(15) 0.0048(12) -0.0088(12) -0.0077(13)
O5 0.0165(19) 0.0127(19) 0.0120(19) 0.000 0.000 -0.0100(17)
O2L 0.0191(15) 0.0196(15) 0.0196(16) 0.0007(12) -0.0053(12) 0.0054(13)
S1 0.0108(4) 0.0157(4) 0.0087(4) -0.0028(3) -0.0010(3) 0.0019(4)
O6 0.0240(15) 0.0139(13) 0.0171(15) -0.0034(11) -0.0028(12) 0.0072(12)
O7 0.0110(14) 0.0330(18) 0.0145(14) -0.0006(12) 0.0026(11) 0.0047(13)
C4 0.0108(16) 0.0134(17) 0.0068(14) -0.0017(12) 0.0005(13) 0.0000(14)
C0AA 0.0162(18) 0.0156(18) 0.0090(17) -0.0001(13) -0.0002(14) -0.0076(16)
C2AA 0.0123(16) 0.0131(16) 0.0105(18) 0.0004(13) -0.0011(13) -0.0058(14)
C7 0.0139(18) 0.0165(19) 0.0138(17) 0.0016(15) -0.0031(14) -0.0020(16)
C6 0.0168(17) 0.0106(15) 0.0187(18) 0.0009(16) -0.0027(17) -0.0021(15)
C5 0.0105(16) 0.0133(17) 0.0104(17) 0.0000(13) 0.0010(13) -0.0040(15)
C3 0.0152(17) 0.0119(17) 0.0112(17) 0.0002(13) -0.0010(14) -0.0008(15)
O2 0.0176(14) 0.0145(14) 0.0168(14) 0.0008(11) -0.0002(11) -0.0063(12)
O1L 0.0210(16) 0.0171(16) 0.0291(18) 0.0082(13) -0.0011(13) 0.0024(13)
O1W 0.039(2) 0.031(2) 0.091(4) -0.001(2) 0.033(3) 0.004(2)
O4 0.0157(13) 0.0151(13) 0.0075(12) -0.0034(10) 0.0012(10) -0.0017(11)
C1 0.060(5) 0.059(5) 0.061(4) -0.004(3) 0.001(3) 0.001(3)
C9 0.046(8) 0.068(8) 0.060(4) -0.004(3) -0.003(3) 0.003(6)
N10 0.034(6) 0.060(8) 0.060(4) -0.005(4) -0.004(4) -0.007(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
Gd1 O1 2.383(3) . y
Gd1 O1 2.470(3) 2_455 y
Gd1 O1 2.409(3) 8_454 y
Gd1 O3 2.352(3) 7_444 y
Gd1 O2L 2.499(3) . y
Gd1 O2 2.342(3) . y
Gd1 O1L 2.448(3) . y
Gd1 O4 2.387(3) 4_464 y
O1 H1 0.71(5) . ?
O3 C0AA 1.257(5) . ?
O5 C5 1.373(4) 2_345 ?
O5 C5 1.373(4) . ?
O2L H2LA 0.81(3) . ?
O2L H2LB 0.86(3) . ?
S1 O6 1.453(3) . ?
S1 O7 1.460(3) . ?
S1 C4 1.776(4) . ?
S1 O4 1.468(3) . ?
C4 C5 1.397(5) . ?
C4 C3 1.390(5) . ?
C0AA C2AA 1.499(5) . ?
C0AA O2 1.268(5) . ?
C2AA C7 1.395(6) . ?
C2AA C3 1.400(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.382(5) . ?
C6 H6 0.9300 . ?
C6 C5 1.389(5) . ?
C3 H3 0.9300 . ?
O1L H1LA 0.83(2) . ?
O1L H1LB 0.85(3) . ?
O1W H1WA 0.8504 . ?
O1W H1WB 0.8507 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C9 1.459(13) . ?
C9 N10 1.29(2) . ?
O0AA H0AA 0.8498 . ?
O0AA H0AB 0.8501 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O1 72.34(11) . 8_454 y
O1 Gd1 O1 66.64(11) . 2_455 y
O1 Gd1 O1 70.84(11) 8_454 2_455 y
O1 Gd1 O2L 124.89(10) 8_454 . y
O1 Gd1 O2L 150.27(10) . . y
O1 Gd1 O2L 138.59(10) 2_455 . y
O1 Gd1 O1L 76.92(10) . . y
O1 Gd1 O1L 131.51(10) 8_454 . y
O1 Gd1 O4 105.10(9) . 4_464 y
O3 Gd1 O1 74.09(10) 7_444 8_454 y
O3 Gd1 O1 99.46(10) 7_444 . y
O3 Gd1 O1 144.75(10) 7_444 2_455 y
O3 Gd1 O2L 67.64(10) 7_444 . y
O3 Gd1 O1L 75.10(12) 7_444 . y
O3 Gd1 O4 138.02(10) 7_444 4_464 y
O2 Gd1 O1 78.91(10) . 2_455 y
O2 Gd1 O1 82.15(10) . 8_454 y
O2 Gd1 O1 142.13(11) . . y
O2 Gd1 O3 99.87(11) . 7_444 y
O2 Gd1 O2L 67.60(11) . . y
O2 Gd1 O1L 139.78(11) . . y
O2 Gd1 O4 80.86(10) . 4_464 y
O1L Gd1 O1 127.77(10) . 2_455 y
O1L Gd1 O2L 73.90(11) . . y
O4 Gd1 O1 77.01(9) 4_464 2_455 y
O4 Gd1 O1 145.91(10) 4_464 8_454 y
O4 Gd1 O2L 74.32(10) 4_464 . y
O4 Gd1 O1L 77.97(11) 4_464 . y
Gd1 O1 Gd1 112.51(11) . 2_455 ?
Gd1 O1 Gd1 104.94(10) . 7_444 ?
Gd1 O1 Gd1 102.31(10) 7_444 2_455 ?
Gd1 O1 H1 122(4) . . ?
Gd1 O1 H1 106(4) 2_455 . ?
Gd1 O1 H1 108(4) 7_444 . ?
C0AA O3 Gd1 126.9(3) . 8_454 ?
C5 O5 C5 118.0(4) . 2_345 ?
Gd1 O2L H2LA 119(3) . . ?
Gd1 O2L H2LB 114(3) . . ?
H2LA O2L H2LB 104(4) . . ?
O6 S1 O7 112.77(19) . . ?
O6 S1 C4 105.56(17) . . ?
O6 S1 O4 112.67(18) . . ?
O7 S1 C4 107.59(18) . . ?
O7 S1 O4 110.83(18) . . ?
O4 S1 C4 106.99(17) . . ?
C5 C4 S1 119.1(3) . . ?
C3 C4 S1 121.5(3) . . ?
C3 C4 C5 119.4(4) . . ?
O3 C0AA C2AA 117.3(4) . . ?
O3 C0AA O2 124.6(4) . . ?
O2 C0AA C2AA 118.1(4) . . ?
C7 C2AA C0AA 118.8(3) . . ?
C7 C2AA C3 119.8(3) . . ?
C3 C2AA C0AA 121.3(3) . . ?
C2AA C7 H7 119.7 . . ?
C6 C7 C2AA 120.7(4) . . ?
C6 C7 H7 119.7 . . ?
C7 C6 H6 120.4 . . ?
C7 C6 C5 119.2(3) . . ?
C5 C6 H6 120.4 . . ?
O5 C5 C4 117.8(3) . . ?
O5 C5 C6 120.9(3) . . ?
C6 C5 C4 121.0(3) . . ?
C4 C3 C2AA 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C2AA C3 H3 120.1 . . ?
C0AA O2 Gd1 137.1(3) . . ?
Gd1 O1L H1LA 125(3) . . ?
Gd1 O1L H1LB 123(3) . . ?
H1LA O1L H1LB 110(5) . . ?
H1WA O1W H1WB 104.4 . . ?
S1 O4 Gd1 145.88(17) . 3_444 ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C9 C1 H1A 109.5 . . ?
C9 C1 H1B 109.5 . . ?
C9 C1 H1C 109.5 . . ?
N10 C9 C1 144(3) . . ?
H0AA O0AA H0AB 104.5 . . ?
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
_geom_hbond_publ_flag
O2L H2LA O6 0.81(3) 2.11(4) 2.766(4) 138(4) 2_355 yes
O2L H2LB O6 0.86(3) 1.94(3) 2.757(4) 160(5) 4_464 yes
O1L H1LA O7 0.83(2) 2.19(3) 3.008(4) 170(5) 2_355 yes
O1L H1LB O1W 0.85(3) 1.89(4) 2.690(5) 157(6) . yes
O1 H1 O1W 0.71(5) 2.45(5) 3.107(6) 155(6) . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O3 C0AA C2AA -173.4(2) 8_454 . . . ?
Gd1 O3 C0AA O2 6.1(6) 8_454 . . . ?
O3 C0AA C2AA C7 4.6(5) . . . . ?
O3 C0AA C2AA C3 -172.0(4) . . . . ?
O3 C0AA O2 Gd1 40.3(6) . . . . ?
S1 C4 C5 O5 9.0(5) . . . . ?
S1 C4 C5 C6 -176.8(3) . . . . ?
S1 C4 C3 C2AA 178.9(3) . . . . ?
O6 S1 C4 C5 -175.9(3) . . . . ?
O6 S1 C4 C3 4.7(4) . . . . ?
O6 S1 O4 Gd1 31.6(4) . . . 3_444 ?
O7 S1 C4 C5 63.5(3) . . . . ?
O7 S1 C4 C3 -116.0(3) . . . . ?
O7 S1 O4 Gd1 159.0(3) . . . 3_444 ?
C4 S1 O4 Gd1 -84.0(3) . . . 3_444 ?
C0AA C2AA C7 C6 -174.9(4) . . . . ?
C0AA C2AA C3 C4 175.0(3) . . . . ?
C2AA C0AA O2 Gd1 -140.2(3) . . . . ?
C2AA C7 C6 C5 0.3(6) . . . . ?
C7 C2AA C3 C4 -1.7(6) . . . . ?
C7 C6 C5 O5 171.5(4) . . . . ?
C7 C6 C5 C4 -2.6(6) . . . . ?
C5 O5 C5 C4 -125.0(4) 2_345 . . . ?
C5 O5 C5 C6 60.7(3) 2_345 . . . ?
C5 C4 C3 C2AA -0.6(6) . . . . ?
C3 C4 C5 O5 -171.6(3) . . . . ?
C3 C4 C5 C6 2.7(6) . . . . ?
C3 C2AA C7 C6 1.8(6) . . . . ?
O2 C0AA C2AA C7 -174.9(4) . . . . ?
O2 C0AA C2AA C3 8.4(6) . . . . ?
O4 S1 C4 C5 -55.6(3) . . . . ?
O4 S1 C4 C3 124.9(3) . . . . ?
loop_
_smtbx_masks_void_content
None
_shelx_res_file
;
TITL SBT2_a.res in I-4
mo_sb17july_0m.res
created by SHELXL-2017/1 at 10:04:31 on 23-Jan-2018
CELL 0.71073 12.9717 12.9717 16.319 90 90 90
ZERR 2 0.0005 0.0005 0.0007 0 0 0
LATT -2
SYMM -X,-Y,+Z
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SFAC C H Gd N O S
UNIT 61.6 90.8 8 2.8 77.2 8
EQIV $1 -2-X,-Y,+Z
EQIV $2 -1-Y,1+X,-1-Z
EQIV $3 +Y,-1-X,-1-Z
EQIV $4 -1-X,1-Y,+Z
DFIX 0.85 O2L H2La O2L H2Lb
DFIX 0.85 O1L H1La O1L H1Lb
DFIX 1.456 0.01 C9 C1
DFIX 2.593 N10 C1
SADI Gd1 H2La Gd1 H2Lb
SADI Gd1 H1La Gd1 H1Lb
DANG 1.34 H2La H2Lb
DANG 1.34 H1La H1Lb
SIMU C1 C9 N10
RIGU C1 C9 N10
RIGU 0.0001 0.0001 N10 C1 C9
ISOR 0.001 0.002 C1
L.S. 20
PLAN 20
TEMP 23
HTAB O1 O1W
HTAB O2L O6_$1
HTAB O2L O6_$2
HTAB O1L O7_$1
HTAB O1L O1W
HTAB O1W O7_$3
HTAB O1W N10
HTAB O1W O0AA_$4
CONN 8 Gd1
BOND $H
CONF
fmap 2
acta
MERG 2
OMIT -3 60
REM
REM
REM >
REM
REM >
REM >
REM
REM
WGHT 0.011300 1.882500
EXTI 0.001764
FVAR 0.07717
GD1 3 -0.652369 0.031354 -0.326883 11.00000 0.00897 0.00770 =
0.00786 -0.00062 -0.00170 0.00074
O1 5 -0.483251 0.101424 -0.314569 11.00000 0.01156 0.00883 =
0.00881 0.00194 0.00156 0.00054
O3 5 -0.658763 -0.245691 -0.243878 11.00000 0.01958 0.01963 =
0.02083 0.00484 -0.00876 -0.00769
O5 5 -1.000000 -0.500000 -0.427061 10.50000 0.01651 0.01272 =
0.01195 0.00000 0.00000 -0.01003
O2L 5 -0.834326 0.045527 -0.375954 11.00000 0.01907 0.01962 =
0.01959 0.00073 -0.00533 0.00540
H2LA 2 -0.858034 0.102678 -0.384266 11.00000 -1.50000
H2LB 2 -0.846466 0.012261 -0.420288 11.00000 -1.50000
S1 6 -1.062591 -0.288319 -0.464624 11.00000 0.01080 0.01566 =
0.00873 -0.00278 -0.00096 0.00190
O6 5 -1.053094 -0.177388 -0.474660 11.00000 0.02402 0.01393 =
0.01715 -0.00341 -0.00283 0.00721
O7 5 -1.157946 -0.318259 -0.423466 11.00000 0.01098 0.03297 =
0.01455 -0.00061 0.00259 0.00467
C4 1 -0.958323 -0.325157 -0.400432 11.00000 0.01081 0.01340 =
0.00678 -0.00175 0.00052 -0.00003
C0AA 1 -0.734911 -0.209368 -0.281749 11.00000 0.01625 0.01563 =
0.00900 -0.00007 -0.00020 -0.00762
C2AA 1 -0.812415 -0.284498 -0.314515 11.00000 0.01225 0.01307 =
0.01046 0.00043 -0.00112 -0.00582
C7 1 -0.800529 -0.388918 -0.296454 11.00000 0.01387 0.01649 =
0.01381 0.00161 -0.00312 -0.00195
AFIX 43
H7 2 -0.748411 -0.409821 -0.261023 11.00000 -1.20000
AFIX 0
C6 1 -0.865387 -0.461616 -0.330660 11.00000 0.01681 0.01060 =
0.01865 0.00086 -0.00271 -0.00211
AFIX 43
H6 2 -0.857359 -0.531135 -0.318274 11.00000 -1.20000
AFIX 0
C5 1 -0.942709 -0.429664 -0.383756 11.00000 0.01052 0.01326 =
0.01042 0.00000 0.00099 -0.00400
C3 1 -0.892624 -0.252481 -0.365962 11.00000 0.01523 0.01194 =
0.01121 0.00017 -0.00097 -0.00081
AFIX 43
H3 2 -0.901917 -0.182771 -0.377042 11.00000 -1.20000
AFIX 0
O2 5 -0.750766 -0.114057 -0.293527 11.00000 0.01756 0.01450 =
0.01682 0.00079 -0.00023 -0.00630
O1L 5 -0.656516 0.179220 -0.420000 11.00000 0.02100 0.01705 =
0.02907 0.00821 -0.00112 0.00239
H1LA 2 -0.702260 0.223406 -0.420731 11.00000 -1.50000
H1LB 2 -0.604357 0.200668 -0.445946 11.00000 -1.50000
AFIX 6
O1W 5 -0.470160 0.254346 -0.460754 11.00000 0.03906 0.03100 =
0.09060 -0.00062 0.03336 0.00381
H1WA 2 -0.428532 0.212029 -0.482867 11.00000 -1.50000
H1WB 2 -0.497134 0.286309 -0.500908 11.00000 -1.50000
AFIX 0
O4 5 -1.050374 -0.344521 -0.542108 11.00000 0.01569 0.01507 =
0.00749 -0.00342 0.00116 -0.00172
PART -1
C1 1 -0.491134 0.505892 -0.267398 10.35000 0.05961 0.05927 =
0.06099 -0.00387 0.00057 0.00081
AFIX 137
H1A 2 -0.544916 0.457147 -0.255922 10.35000 -1.50000
H1B 2 -0.514626 0.574126 -0.254355 10.35000 -1.50000
H1C 2 -0.431608 0.489790 -0.234871 10.35000 -1.50000
AFIX 0
C9 1 -0.464162 0.500746 -0.354081 10.35000 0.04573 0.06792 =
0.06004 -0.00409 -0.00317 0.00270
N10 4 -0.414265 0.448271 -0.408055 10.35000 0.03409 0.06003 =
0.06036 -0.00549 -0.00413 -0.00735
PART 0
PART -2
O0AA 5 -0.433811 0.498874 -0.417934 10.15000 0.11184
AFIX 3
H0AA 2 -0.483501 0.504714 -0.384314 10.15000 -1.50000
H0AB 2 -0.386171 0.470024 -0.390474 10.15000 -1.50000
AFIX 0
PART 0
H1 2 -0.466638 0.143128 -0.339129 11.00000 0.02526
HKLF 4
REM SBT2_a.res in I-4
REM R1 = 0.0180 for 3943 Fo > 4sig(Fo) and 0.0186 for all 4010 data
REM 220 parameters refined using 37 restraints
END
WGHT 0.0113 1.8806
REM Highest difference peak 0.706, deepest hole -0.864, 1-sigma level 0.097
Q1 1 -0.6521 0.0297 -0.2791 11.00000 0.05 0.71
Q2 1 -0.6516 0.0309 -0.3771 11.00000 0.05 0.64
Q3 1 -0.5980 0.0736 -0.2869 11.00000 0.05 0.62
Q4 1 -0.5976 -0.0131 -0.2866 11.00000 0.05 0.57
Q5 1 -0.7032 0.0769 -0.2862 11.00000 0.05 0.56
Q6 1 -0.7066 -0.0121 -0.2884 11.00000 0.05 0.56
Q7 1 -0.5974 -0.0129 -0.3643 11.00000 0.05 0.55
Q8 1 -0.5951 0.0724 -0.3642 11.00000 0.05 0.53
Q9 1 -0.4994 0.5387 -0.2868 11.00000 0.05 0.52
Q10 1 -0.7040 -0.0088 -0.3630 11.00000 0.05 0.50
Q11 1 -0.4674 0.4980 -0.2439 11.00000 0.05 0.48
Q12 1 -0.4929 0.2514 -0.5103 11.00000 0.05 0.46
Q13 1 -0.5585 0.1142 -0.3229 11.00000 0.05 0.45
Q14 1 -0.4342 0.0616 -0.3207 11.00000 0.05 0.44
Q15 1 -0.7060 0.0733 -0.3689 11.00000 0.05 0.43
Q16 1 -0.7575 0.0316 -0.2931 11.00000 0.05 0.41
Q17 1 -0.4722 0.1473 -0.4846 11.00000 0.05 0.39
Q18 1 -0.7193 -0.2732 -0.3290 11.00000 0.05 0.38
Q19 1 -0.4438 0.5425 -0.4291 11.00000 0.05 0.35
Q20 1 -1.0721 -0.2950 -0.5108 11.00000 0.05 0.35
;
_shelx_res_checksum 55306
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_CP_4
_database_code_depnum_ccdc_archive 'CCDC 1838577'
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-10-02 downloaded from the CCDC.
;
_audit_creation_date 2018-01-23
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H32 Er4 O34 S4, 4.6(H2 O), 1.4(C2 H3 N1)'
_chemical_formula_sum 'C30.80 H45.40 Er4 N1.40 O38.60 S4'
_chemical_formula_weight 1850.16
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Er Er -0.2586 4.9576 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system tetragonal
_space_group_IT_number 82
_space_group_name_H-M_alt 'I -4'
_space_group_name_Hall 'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-y, x, -z'
'-x, -y, z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
_cell_length_a 12.8363(2)
_cell_length_b 12.8363(2)
_cell_length_c 16.2028(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2669.75(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6992
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 36.381
_cell_measurement_theta_min 2.244
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 6.487
_exptl_absorpt_correction_T_max 0.7471
_exptl_absorpt_correction_T_min 0.5058
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0965 before and 0.0524 after correction. The Ratio of minimum to maximum transmission is 0.6770. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'pale pink'
_exptl_crystal_density_diffrn 2.302
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1770
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.22
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0217
_diffrn_reflns_av_unetI/netI 0.0416
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 9888
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.979
_diffrn_reflns_theta_min 2.024
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.895
_reflns_Friedel_fraction_full 0.985
_reflns_Friedel_fraction_max 0.961
_reflns_number_gt 3716
_reflns_number_total 3819
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.760
_refine_diff_density_min -0.680
_refine_diff_density_rms 0.114
_refine_ls_abs_structure_details
;
Flack x determined using 1673 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.012(6)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 215
_refine_ls_number_reflns 3819
_refine_ls_number_restraints 37
_refine_ls_R_factor_all 0.0226
_refine_ls_R_factor_gt 0.0216
_refine_ls_restrained_S_all 1.016
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0406
_refine_ls_wR_factor_ref 0.0410
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All O(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
O2L-H2LA = O2L-H2LB
0.85 with sigma of 0.02
O1L-H1LA = O1L-H1LB
0.85 with sigma of 0.02
C9-C1AA
1.456 with sigma of 0.01
N10-C1AA
2.593 with sigma of 0.02
H2LA-H2LB
1.34 with sigma of 0.04
H1LA-H1LB
1.34 with sigma of 0.04
Er1-H2LA \\sim Er1-H2LB
with sigma of 0.02
Er1-H1LA \\sim Er1-H1LB
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1AA \\sim C9 \\sim N10: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C1AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
C1AA, C9, N10
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
N10, C1AA, C9
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
Fixed Sof: C1AA(0.35) HB(0.35) HC(0.35) HD(0.35) C9(0.35) N10(0.35)
O0AA(0.15) HE(0.15) HF(0.15)
6.a Riding coordinates:
O0AA(HE,HF)
6.b Free rotating group:
O1W(H,HA)
6.c Ternary CH refined with riding coordinates:
O1(H1)
6.d Aromatic/amide H refined with riding coordinates:
C7(H7), C6(H6), C3(H3)
6.e Idealised Me refined as rotating group:
C1AA(HB,HC,HD)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.65001(2) -0.03218(2) 0.32612(2) 0.00937(5) Uani 1 1 d D . . . .
O1 O 0.4827(2) -0.1006(2) 0.3138(2) 0.0104(7) Uani 1 1 d . . . . .
H1 H 0.470783 -0.159141 0.351490 0.012 Uiso 1 1 calc R . . . .
O3 O 0.6588(3) 0.2409(3) 0.2435(3) 0.0215(9) Uani 1 1 d . . . . .
O5 O 1.000000 0.500000 0.4291(4) 0.0145(12) Uani 1 2 d S T P . .
O2L O 0.8301(3) -0.0517(3) 0.3738(3) 0.0238(10) Uani 1 1 d D . . . .
H2LA H 0.852(4) -0.109(3) 0.388(4) 0.036 Uiso 1 1 d DR . . . .
H2LB H 0.847(4) -0.016(4) 0.418(3) 0.036 Uiso 1 1 d DR . . . .
S1 S 1.06275(10) 0.28691(10) 0.46868(9) 0.0142(3) Uani 1 1 d . . . . .
O6 O 1.0525(3) 0.1753(3) 0.4800(3) 0.0216(9) Uani 1 1 d . . . . .
O7 O 1.1590(3) 0.3153(3) 0.4274(3) 0.0221(10) Uani 1 1 d . . . . .
C4 C 0.9586(4) 0.3241(4) 0.4022(3) 0.0110(10) Uani 1 1 d . . . . .
C0AA C 0.7360(4) 0.2047(4) 0.2817(4) 0.0150(11) Uani 1 1 d . . . . .
C2AA C 0.8126(4) 0.2811(4) 0.3154(4) 0.0130(11) Uani 1 1 d . . . . .
C7 C 0.8009(4) 0.3860(4) 0.2971(4) 0.0162(12) Uani 1 1 d . . . . .
H7 H 0.748930 0.406965 0.260712 0.019 Uiso 1 1 calc R . . . .
C6 C 0.8658(4) 0.4601(4) 0.3326(4) 0.0164(11) Uani 1 1 d . . . . .
H6 H 0.857051 0.530350 0.320410 0.020 Uiso 1 1 calc R . . . .
C5 C 0.9426(4) 0.4290(4) 0.3855(3) 0.0130(11) Uani 1 1 d . . . . .
C3 C 0.8933(4) 0.2510(4) 0.3679(4) 0.0139(11) Uani 1 1 d . . . . .
H3 H 0.903138 0.180763 0.379815 0.017 Uiso 1 1 calc R . . . .
O2 O 0.7519(3) 0.1086(3) 0.2944(3) 0.0177(9) Uani 1 1 d . . . . .
O1L O 0.6515(3) -0.1767(3) 0.4188(3) 0.0241(10) Uani 1 1 d D . . . .
H1LA H 0.702(3) -0.217(4) 0.420(4) 0.036 Uiso 1 1 d DR . . . .
H1LB H 0.597(3) -0.197(4) 0.441(4) 0.036 Uiso 1 1 d DR . . . .
O1W O 0.4675(4) -0.2573(4) 0.4592(4) 0.0544(18) Uani 1 1 d . . . . .
H H 0.444903 -0.233469 0.504247 0.082 Uiso 1 1 d G . . . .
HA H 0.477599 -0.321005 0.468631 0.082 Uiso 1 1 d G . . . .
O4 O 1.0503(3) 0.3450(3) 0.5455(2) 0.0138(8) Uani 1 1 d . . . . .
C1AA C 0.494(5) -0.497(7) 0.2643(12) 0.054(6) Uani 0.35 1 d D U . A -1
HB H 0.472810 -0.430184 0.242942 0.080 Uiso 0.35 1 calc GR . . A -1
HC H 0.457329 -0.550923 0.235111 0.080 Uiso 0.35 1 calc GR . . A -1
HD H 0.567234 -0.505528 0.257171 0.080 Uiso 0.35 1 calc GR . . A -1
C9 C 0.4680(14) -0.503(2) 0.3514(12) 0.045(5) Uani 0.35 1 d D U . A -1
N10 N 0.4180(16) -0.4602(18) 0.4108(15) 0.065(6) Uani 0.35 1 d D U . A -1
O0AA O 0.449(4) -0.522(4) 0.420(3) 0.077(16) Uiso 0.15 1 d . . . B -2
HE H 0.498563 -0.527822 0.386722 0.115 Uiso 0.15 1 d R . . B -2
HF H 0.401203 -0.493152 0.392882 0.115 Uiso 0.15 1 d R . . B -2
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
Er1 0.01103(11) 0.00894(11) 0.00813(10) -0.00073(10) -0.00185(10) 0.00085(8)
O1 0.0127(15) 0.0109(15) 0.007(2) 0.0039(14) 0.0023(15) 0.0006(12)
O3 0.021(2) 0.026(2) 0.017(2) 0.0057(18) -0.0100(18) -0.0104(16)
O5 0.016(3) 0.014(3) 0.014(3) 0.000 0.000 -0.009(2)
O2L 0.025(2) 0.023(2) 0.023(3) 0.000(2) -0.009(2) 0.0061(17)
S1 0.0125(6) 0.0206(7) 0.0095(7) -0.0045(6) -0.0013(5) 0.0042(5)
O6 0.028(2) 0.0182(19) 0.018(2) -0.0046(18) -0.0057(19) 0.0102(16)
O7 0.011(2) 0.042(3) 0.014(2) -0.002(2) 0.0017(17) 0.0079(17)
C4 0.011(2) 0.016(2) 0.006(2) -0.0018(19) 0.000(2) 0.0021(18)
C0AA 0.018(3) 0.019(3) 0.008(3) -0.002(2) 0.000(2) -0.008(2)
C2AA 0.012(2) 0.018(2) 0.008(3) -0.002(2) 0.000(2) -0.0079(18)
C7 0.015(2) 0.020(3) 0.014(3) 0.002(2) -0.006(2) -0.001(2)
C6 0.018(2) 0.013(2) 0.018(3) 0.002(3) -0.002(3) -0.0044(17)
C5 0.013(2) 0.017(3) 0.009(3) -0.001(2) 0.004(2) -0.0060(18)
C3 0.019(3) 0.014(3) 0.009(3) 0.000(2) 0.001(2) -0.001(2)
O2 0.020(2) 0.0172(19) 0.016(2) 0.0010(17) -0.0020(17) -0.0062(15)
O1L 0.023(2) 0.020(2) 0.029(3) 0.009(2) -0.002(2) 0.0005(17)
O1W 0.046(3) 0.029(3) 0.088(6) -0.001(3) 0.038(3) 0.005(2)
O4 0.0151(18) 0.0171(18) 0.009(2) -0.0028(16) 0.0007(16) -0.0015(14)
C1AA 0.053(6) 0.053(6) 0.054(6) 0.000(3) 0.000(3) 0.001(3)
C9 0.030(11) 0.043(11) 0.064(11) -0.011(10) -0.007(9) 0.012(12)
N10 0.048(13) 0.056(14) 0.090(15) -0.030(13) 0.010(11) -0.010(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
Er1 O1 2.329(3) . y
Er1 O1 2.418(3) 4_655 y
Er1 O1 2.362(4) 7_545 y
Er1 O3 2.296(4) 6 y
Er1 O2L 2.450(4) . y
Er1 O2 2.290(4) . y
Er1 O1L 2.387(4) . y
Er1 O4 2.335(4) 3_646 y
O1 H1 0.9800 . ?
O3 C0AA 1.258(6) . ?
O5 C5 1.369(6) . ?
O5 C5 1.368(6) 4_765 ?
O2L H2LA 0.82(3) . ?
O2L H2LB 0.88(3) . ?
S1 O6 1.451(4) . ?
S1 O7 1.451(4) . ?
S1 C4 1.783(6) . ?
S1 O4 1.460(4) . ?
C4 C5 1.388(7) . ?
C4 C3 1.375(7) . ?
C0AA C2AA 1.492(7) . ?
C0AA O2 1.266(6) . ?
C2AA C7 1.387(7) . ?
C2AA C3 1.395(7) . ?
C7 H7 0.9300 . ?
C7 C6 1.389(7) . ?
C6 H6 0.9300 . ?
C6 C5 1.366(8) . ?
C3 H3 0.9300 . ?
O1L H1LA 0.82(3) . ?
O1L H1LB 0.82(3) . ?
O1W H 0.8432 . ?
O1W HA 0.8423 . ?
C1AA HB 0.9600 . ?
C1AA HC 0.9600 . ?
C1AA HD 0.9600 . ?
C1AA C9 1.451(13) . ?
C9 N10 1.28(3) . ?
O0AA HE 0.8423 . ?
O0AA HF 0.8421 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Er1 O1 72.59(14) . 7_545 y
O1 Er1 O1 66.99(12) . 4_655 y
O1 Er1 O1 71.03(14) 7_545 4_655 y
O1 Er1 O2L 124.35(14) 7_545 . y
O1 Er1 O2L 149.15(13) . . y
O1 Er1 O2L 139.70(12) 4_655 . y
O1 Er1 O1L 76.60(13) . . y
O1 Er1 O1L 131.99(14) 7_545 . y
O1 Er1 O4 105.81(13) . 3_646 y
O3 Er1 O1 73.88(13) 6 7_545 y
O3 Er1 O1 99.17(13) 6 . y
O3 Er1 O1 144.72(14) 6 4_655 y
O3 Er1 O2L 66.62(14) 6 . y
O3 Er1 O1L 75.80(16) 6 . y
O3 Er1 O4 138.12(13) 6 3_646 y
O2 Er1 O1 80.07(12) . 4_655 y
O2 Er1 O1 82.77(13) . 7_545 y
O2 Er1 O1 143.65(13) . . y
O2 Er1 O3 99.11(14) . 6 y
O2 Er1 O2L 67.20(14) . . y
O2 Er1 O1L 138.61(14) . . y
O2 Er1 O4 80.00(14) . 3_646 y
O1L Er1 O1 127.25(14) . 4_655 y
O1L Er1 O2L 73.42(14) . . y
O4 Er1 O1 76.87(12) 3_646 4_655 y
O4 Er1 O1 145.67(12) 3_646 7_545 y
O4 Er1 O2L 74.91(14) 3_646 . y
O4 Er1 O1L 77.98(15) 3_646 . y
Er1 O1 Er1 112.13(12) . 4_655 ?
Er1 O1 Er1 104.94(13) . 6 ?
Er1 O1 Er1 102.21(13) 6 4_655 ?
Er1 O1 H1 112.3 . . ?
Er1 O1 H1 112.3 4_655 . ?
Er1 O1 H1 112.3 6 . ?
C0AA O3 Er1 127.7(3) . 7_545 ?
C5 O5 C5 117.9(6) 4_765 . ?
Er1 O2L H2LA 121(3) . . ?
Er1 O2L H2LB 115(3) . . ?
H2LA O2L H2LB 99(5) . . ?
O6 S1 O7 112.5(3) . . ?
O6 S1 C4 105.9(2) . . ?
O6 S1 O4 112.8(3) . . ?
O7 S1 C4 107.0(3) . . ?
O7 S1 O4 111.0(2) . . ?
O4 S1 C4 107.3(2) . . ?
C5 C4 S1 119.2(4) . . ?
C3 C4 S1 121.2(4) . . ?
C3 C4 C5 119.6(5) . . ?
O3 C0AA C2AA 117.1(5) . . ?
O3 C0AA O2 124.5(5) . . ?
O2 C0AA C2AA 118.3(5) . . ?
C7 C2AA C0AA 119.2(5) . . ?
C7 C2AA C3 118.7(4) . . ?
C3 C2AA C0AA 122.0(5) . . ?
C2AA C7 H7 119.6 . . ?
C2AA C7 C6 120.7(5) . . ?
C6 C7 H7 119.6 . . ?
C7 C6 H6 120.3 . . ?
C5 C6 C7 119.5(5) . . ?
C5 C6 H6 120.3 . . ?
O5 C5 C4 117.8(5) . . ?
C6 C5 O5 121.2(4) . . ?
C6 C5 C4 120.8(5) . . ?
C4 C3 C2AA 120.6(5) . . ?
C4 C3 H3 119.7 . . ?
C2AA C3 H3 119.7 . . ?
C0AA O2 Er1 135.5(3) . . ?
Er1 O1L H1LA 121(3) . . ?
Er1 O1L H1LB 121(3) . . ?
H1LA O1L H1LB 117(5) . . ?
H O1W HA 104.3 . . ?
S1 O4 Er1 145.4(2) . 2_666 ?
HB C1AA HC 109.5 . . ?
HB C1AA HD 109.5 . . ?
HC C1AA HD 109.5 . . ?
C9 C1AA HB 109.5 . . ?
C9 C1AA HC 109.5 . . ?
C9 C1AA HD 109.5 . . ?
N10 C9 C1AA 146(4) . . ?
HE O0AA HF 104.3 . . ?
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
_geom_hbond_publ_flag
O1 H1 O1W 0.98 2.15 3.103(7) 163.1 . yes
O1L H1LB O1W 0.82(3) 1.86(3) 2.660(7) 163(7) . yes
O1W HA N10 0.84 2.16 2.79(2) 132.1 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Er1 O3 C0AA C2AA 174.5(3) 7_545 . . . ?
Er1 O3 C0AA O2 -6.6(8) 7_545 . . . ?
O3 C0AA C2AA C7 -5.7(8) . . . . ?
O3 C0AA C2AA C3 171.4(5) . . . . ?
O3 C0AA O2 Er1 -38.6(9) . . . . ?
S1 C4 C5 O5 -7.8(7) . . . . ?
S1 C4 C5 C6 177.7(4) . . . . ?
S1 C4 C3 C2AA -179.5(4) . . . . ?
O6 S1 C4 C5 174.6(4) . . . . ?
O6 S1 C4 C3 -4.8(5) . . . . ?
O6 S1 O4 Er1 -31.8(5) . . . 2_666 ?
O7 S1 C4 C5 -65.2(5) . . . . ?
O7 S1 C4 C3 115.5(5) . . . . ?
O7 S1 O4 Er1 -159.1(4) . . . 2_666 ?
C4 S1 O4 Er1 84.4(4) . . . 2_666 ?
C0AA C2AA C7 C6 175.0(5) . . . . ?
C0AA C2AA C3 C4 -175.8(5) . . . . ?
C2AA C0AA O2 Er1 140.3(4) . . . . ?
C2AA C7 C6 C5 0.6(9) . . . . ?
C7 C2AA C3 C4 1.4(8) . . . . ?
C7 C6 C5 O5 -172.3(5) . . . . ?
C7 C6 C5 C4 2.1(9) . . . . ?
C5 O5 C5 C4 125.0(5) 4_765 . . . ?
C5 O5 C5 C6 -60.5(5) 4_765 . . . ?
C5 C4 C3 C2AA 1.2(8) . . . . ?
C3 C4 C5 O5 171.6(5) . . . . ?
C3 C4 C5 C6 -3.0(8) . . . . ?
C3 C2AA C7 C6 -2.3(8) . . . . ?
O2 C0AA C2AA C7 175.3(5) . . . . ?
O2 C0AA C2AA C3 -7.6(8) . . . . ?
O4 S1 C4 C5 53.9(5) . . . . ?
O4 S1 C4 C3 -125.4(4) . . . . ?
loop_
_smtbx_masks_void_content
''
_shelx_res_file
;
TITL TR2 in I-4
sb158_0m.res
created by SHELXL-2017/1 at 10:33:19 on 23-Jan-2018
CELL 0.71073 12.8363 12.8363 16.2028 90 90 90
ZERR 2 0.0002 0.0002 0.0004 0 0 0
LATT -2
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SYMM -X,-Y,+Z
SFAC C H Er N O S
UNIT 61.6 90.8 8 2.8 77.2 8
DFIX 0.85 O2L H2La O2L H2Lb
DFIX 0.85 O1L H1La O1L H1Lb
DFIX 1.456 0.01 C9 C1AA
DFIX 2.593 N10 C1AA
SADI Er1 H2La Er1 H2Lb
SADI Er1 H1La Er1 H1Lb
DANG 1.34 H2La H2Lb
DANG 1.34 H1La H1Lb
SIMU C1AA C9 N10
RIGU C1AA C9 N10
RIGU 0.01 0.01 N10 C1AA C9
ISOR 0.001 0.002 C1AA
L.S. 20
PLAN 20
TEMP 23
HTAB O1 O1W
HTAB O1L O1W
HTAB O1W N10
CONN 8 Er1
BOND $H
CONF
fmap 2
acta
MERG 2
OMIT -3 60
REM
REM
REM >
REM
REM >
REM >
REM
REM
WGHT 0.011300
FVAR 0.21575
ER1 3 0.650012 -0.032182 0.326116 11.00000 0.01103 0.00894 =
0.00813 -0.00073 -0.00185 0.00085
O1 5 0.482673 -0.100608 0.313818 11.00000 0.01272 0.01089 =
0.00744 0.00391 0.00234 0.00063
AFIX 13
H1 2 0.470783 -0.159141 0.351490 11.00000 -1.20000
AFIX 0
O3 5 0.658823 0.240870 0.243454 11.00000 0.02144 0.02565 =
0.01737 0.00566 -0.01000 -0.01045
O5 5 1.000000 0.500000 0.429068 10.50000 0.01607 0.01400 =
0.01354 0.00000 0.00000 -0.00910
O2L 5 0.830102 -0.051697 0.373793 11.00000 0.02470 0.02343 =
0.02323 -0.00017 -0.00879 0.00611
H2LA 2 0.852486 -0.109000 0.388351 11.00000 -1.50000
H2LB 2 0.846609 -0.015619 0.418322 11.00000 -1.50000
S1 6 1.062746 0.286909 0.468676 11.00000 0.01248 0.02055 =
0.00950 -0.00450 -0.00126 0.00419
O6 5 1.052547 0.175269 0.479999 11.00000 0.02833 0.01820 =
0.01828 -0.00457 -0.00566 0.01023
O7 5 1.158957 0.315281 0.427379 11.00000 0.01055 0.04193 =
0.01391 -0.00171 0.00173 0.00790
C4 1 0.958559 0.324143 0.402181 11.00000 0.01062 0.01612 =
0.00641 -0.00182 -0.00030 0.00214
C0AA 1 0.736032 0.204659 0.281720 11.00000 0.01783 0.01931 =
0.00776 -0.00166 0.00047 -0.00752
C2AA 1 0.812606 0.281097 0.315419 11.00000 0.01201 0.01838 =
0.00848 -0.00153 -0.00027 -0.00785
C7 1 0.800857 0.386001 0.297131 11.00000 0.01481 0.01994 =
0.01396 0.00224 -0.00638 -0.00135
AFIX 43
H7 2 0.748930 0.406965 0.260712 11.00000 -1.20000
AFIX 0
C6 1 0.865778 0.460092 0.332600 11.00000 0.01813 0.01311 =
0.01806 0.00206 -0.00246 -0.00436
AFIX 43
H6 2 0.857051 0.530350 0.320410 11.00000 -1.20000
AFIX 0
C5 1 0.942555 0.428959 0.385533 11.00000 0.01290 0.01696 =
0.00911 -0.00099 0.00434 -0.00600
C3 1 0.893338 0.250956 0.367904 11.00000 0.01899 0.01367 =
0.00902 -0.00019 0.00090 -0.00060
AFIX 43
H3 2 0.903138 0.180763 0.379815 11.00000 -1.20000
AFIX 0
O2 5 0.751931 0.108624 0.294383 11.00000 0.01962 0.01723 =
0.01628 0.00099 -0.00197 -0.00621
O1L 5 0.651498 -0.176690 0.418828 11.00000 0.02335 0.01985 =
0.02924 0.00870 -0.00178 0.00048
H1LA 2 0.701602 -0.216886 0.420167 11.00000 -1.50000
H1LB 2 0.597098 -0.197015 0.440636 11.00000 -1.50000
AFIX 6
O1W 5 0.467491 -0.257276 0.459169 11.00000 0.04626 0.02901 =
0.08787 -0.00126 0.03790 0.00456
H 2 0.444903 -0.233469 0.504247 11.00000 -1.50000
HA 2 0.477599 -0.321005 0.468631 11.00000 -1.50000
AFIX 0
O4 5 1.050340 0.345017 0.545517 11.00000 0.01506 0.01709 =
0.00922 -0.00282 0.00065 -0.00155
PART -1
C1AA 1 0.493502 -0.496810 0.264289 10.35000 0.05345 0.05281 =
0.05444 -0.00008 -0.00030 0.00086
AFIX 137
HB 2 0.472810 -0.430184 0.242942 10.35000 -1.50000
HC 2 0.457329 -0.550923 0.235111 10.35000 -1.50000
HD 2 0.567234 -0.505528 0.257171 10.35000 -1.50000
AFIX 0
C9 1 0.468012 -0.502543 0.351397 10.35000 0.02962 0.04274 =
0.06372 -0.01075 -0.00742 0.01188
N10 4 0.417983 -0.460183 0.410830 10.35000 0.04766 0.05627 =
0.08992 -0.03004 0.00999 -0.01027
PART 0
PART -2
O0AA 5 0.448853 -0.521992 0.420342 10.15000 0.07692
AFIX 3
HE 2 0.498563 -0.527822 0.386722 10.15000 -1.50000
HF 2 0.401203 -0.493152 0.392882 10.15000 -1.50000
AFIX 0
HKLF 4
REM TR2 in I-4
REM R1 = 0.0216 for 3716 Fo > 4sig(Fo) and 0.0226 for all 3819 data
REM 215 parameters refined using 37 restraints
END
WGHT 0.0113 0.0000
REM Highest difference peak 0.760, deepest hole -0.680, 1-sigma level 0.114
Q1 1 0.6461 -0.0259 0.2715 11.00000 0.05 0.76
Q2 1 0.6636 -0.0228 0.3813 11.00000 0.05 0.68
Q3 1 0.5985 0.0123 0.3292 11.00000 0.05 0.56
Q4 1 0.7122 -0.0658 0.3214 11.00000 0.05 0.56
Q5 1 0.3988 -0.4563 0.4689 11.00000 0.05 0.56
Q6 1 0.6200 -0.0902 0.3274 11.00000 0.05 0.55
Q7 1 0.5448 -0.4898 0.2449 11.00000 0.05 0.53
Q8 1 0.4606 -0.1392 0.2771 11.00000 0.05 0.44
Q9 1 0.9656 0.3551 0.3656 11.00000 0.05 0.39
Q10 1 0.9662 0.3572 0.5752 11.00000 0.05 0.39
Q11 1 0.6141 -0.0453 0.3689 11.00000 0.05 0.39
Q12 1 0.4852 -0.2500 0.5107 11.00000 0.05 0.38
Q13 1 0.4959 -0.4528 0.2782 11.00000 0.05 0.38
Q14 1 0.4216 -0.5466 0.3453 11.00000 0.05 0.37
Q15 1 0.4626 -0.4476 0.1724 11.00000 0.05 0.37
Q16 1 0.7882 0.2428 0.2893 11.00000 0.05 0.36
Q17 1 0.9376 0.1031 0.4367 11.00000 0.05 0.36
Q18 1 0.5000 -0.5000 0.2095 10.50000 0.05 0.36
Q19 1 0.5000 -0.5000 0.3018 10.50000 0.05 0.35
Q20 1 0.4405 -0.4595 0.3300 11.00000 0.05 0.35
;
_shelx_res_checksum 20703
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_CP_3
_database_code_depnum_ccdc_archive 'CCDC 1838576'
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-10-02 downloaded from the CCDC.
;
_audit_creation_date 2018-01-23
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H32 Ho4 O34 S84, 4.6(H2 O), 1.4(C2 H3 N1)'
_chemical_formula_sum 'C30.80 H45.40 Ho4 N1.40 O38.60 S4'
_chemical_formula_weight 1840.84
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Ho Ho -0.2175 4.6783 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system tetragonal
_space_group_IT_number 82
_space_group_name_H-M_alt 'I -4'
_space_group_name_Hall 'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-y, x, -z'
'-x, -y, z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
_cell_length_a 12.8759(6)
_cell_length_b 12.8759(6)
_cell_length_c 16.2369(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2691.9(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6681
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 33.288
_cell_measurement_theta_min 3.364
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 6.077
_exptl_absorpt_correction_T_max 0.7465
_exptl_absorpt_correction_T_min 0.5159
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0931 before and 0.0502 after correction. The Ratio of minimum to maximum transmission is 0.6911. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'pale pink'
_exptl_crystal_density_diffrn 2.271
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1762
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.31
_exptl_crystal_size_min 0.28
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0219
_diffrn_reflns_av_unetI/netI 0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 7832
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.990
_diffrn_reflns_theta_min 2.509
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.700
_reflns_Friedel_fraction_full 0.828
_reflns_Friedel_fraction_max 0.748
_reflns_number_gt 3368
_reflns_number_total 3441
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.749
_refine_diff_density_min -0.595
_refine_diff_density_rms 0.112
_refine_ls_abs_structure_details
;
Flack x determined using 1337 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.039(6)
_refine_ls_extinction_coef 0.00024(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref 1.004
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 216
_refine_ls_number_reflns 3441
_refine_ls_number_restraints 37
_refine_ls_R_factor_all 0.0208
_refine_ls_R_factor_gt 0.0201
_refine_ls_restrained_S_all 1.000
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0073P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0395
_refine_ls_wR_factor_ref 0.0397
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All O(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
O2L-H2LA = O2L-H2LB
0.85 with sigma of 0.02
O1L-H1LA = O1L-H1LB
0.85 with sigma of 0.02
C9-C1AA
1.456 with sigma of 0.01
N10-C1AA
2.593 with sigma of 0.02
H2LA-H2LB
1.34 with sigma of 0.04
H1LA-H1LB
1.34 with sigma of 0.04
Ho1-H2LA \\sim Ho1-H2LB
with sigma of 0.02
Ho1-H1LA \\sim Ho1-H1LB
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1AA \\sim C9 \\sim N10: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C1AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
C1AA, C9, N10
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
N10, C1AA, C9
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
Fixed Sof: C1AA(0.35) HB(0.35) HC(0.35) HD(0.35) C9(0.35) N10(0.35)
O0AA(0.15) HE(0.15) HF(0.15)
6.a Riding coordinates:
O0AA(HE,HF)
6.b Free rotating group:
O1W(H,HA)
6.c Ternary CH refined with riding coordinates:
O1(H1)
6.d Aromatic/amide H refined with riding coordinates:
C7(H7), C6(H6), C3(H3)
6.e Idealised Me refined as rotating group:
C1AA(HB,HC,HD)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.65105(2) -0.03169(2) 0.32651(2) 0.00899(6) Uani 1 1 d D . . . .
O1 O 0.4827(2) -0.1011(2) 0.31417(19) 0.0082(7) Uani 1 1 d . . . . .
H1 H 0.471082 -0.159446 0.351789 0.010 Uiso 1 1 calc R . . . .
O3 O 0.6586(3) 0.2433(3) 0.2436(2) 0.0189(9) Uani 1 1 d . . . . .
O5 O 1.000000 0.500000 0.4277(3) 0.0118(11) Uani 1 2 d S T P . .
O2L O 0.8321(3) -0.0482(3) 0.3751(2) 0.0189(9) Uani 1 1 d D . . . .
H2LA H 0.857(3) -0.106(2) 0.383(4) 0.028 Uiso 1 1 d DR . . . .
H2LB H 0.848(4) -0.014(4) 0.419(3) 0.028 Uiso 1 1 d DR . . . .
S1 S 1.06290(10) 0.28779(10) 0.46653(8) 0.0118(3) Uani 1 1 d . . . . .
O6 O 1.0527(3) 0.1763(3) 0.4772(2) 0.0189(8) Uani 1 1 d . . . . .
O7 O 1.1586(3) 0.3169(3) 0.4253(2) 0.0195(9) Uani 1 1 d . . . . .
C4 C 0.9584(4) 0.3247(4) 0.4015(3) 0.0093(10) Uani 1 1 d . . . . .
C0AA C 0.7356(4) 0.2068(4) 0.2819(3) 0.0147(11) Uani 1 1 d . . . . .
C2AA C 0.8127(4) 0.2830(4) 0.3148(3) 0.0106(10) Uani 1 1 d . . . . .
C7 C 0.8007(4) 0.3867(4) 0.2971(3) 0.0150(11) Uani 1 1 d . . . . .
H7 H 0.748283 0.407484 0.261356 0.018 Uiso 1 1 calc R . . . .
C6 C 0.8657(4) 0.4611(4) 0.3318(4) 0.0144(10) Uani 1 1 d . . . . .
H6 H 0.857209 0.531041 0.319274 0.017 Uiso 1 1 calc R . . . .
C5 C 0.9424(4) 0.4294(4) 0.3847(3) 0.0102(10) Uani 1 1 d . . . . .
C3 C 0.8930(4) 0.2520(4) 0.3668(3) 0.0126(11) Uani 1 1 d . . . . .
H3 H 0.902593 0.181858 0.378161 0.015 Uiso 1 1 calc R . . . .
O2 O 0.7517(3) 0.1115(3) 0.2940(2) 0.0156(8) Uani 1 1 d . . . . .
O1L O 0.6543(3) -0.1774(3) 0.4191(3) 0.0215(10) Uani 1 1 d D . . . .
H1LA H 0.703(3) -0.219(3) 0.418(4) 0.032 Uiso 1 1 d DR . . . .
H1LB H 0.601(3) -0.200(4) 0.440(4) 0.032 Uiso 1 1 d DR . . . .
O1W O 0.4681(4) -0.2553(4) 0.4598(4) 0.0506(16) Uani 1 1 d . . . . .
H H 0.484200 -0.244350 0.509490 0.076 Uiso 1 1 d G . . . .
HA H 0.456037 -0.319754 0.457694 0.076 Uiso 1 1 d G . . . .
O4 O 1.0503(3) 0.3445(3) 0.5434(2) 0.0120(8) Uani 1 1 d . . . . .
C1AA C 0.495(4) -0.503(6) 0.2668(10) 0.048(5) Uani 0.35 1 d D U . A -1
HB H 0.545105 -0.449156 0.257205 0.073 Uiso 0.35 1 calc GR . . A -1
HC H 0.435449 -0.491896 0.232477 0.073 Uiso 0.35 1 calc GR . . A -1
HD H 0.525496 -0.569248 0.253931 0.073 Uiso 0.35 1 calc GR . . A -1
C9 C 0.4636(14) -0.502(2) 0.3531(10) 0.041(5) Uani 0.35 1 d D U . A -1
N10 N 0.4170(14) -0.4555(16) 0.4097(12) 0.047(4) Uani 0.35 1 d D U . A -1
O0AA O 0.442(3) -0.523(3) 0.422(3) 0.059(12) Uiso 0.15 1 d . . . B -2
HE H 0.491928 -0.528815 0.388106 0.088 Uiso 0.15 1 d R . . B -2
HF H 0.394568 -0.494115 0.394266 0.088 Uiso 0.15 1 d R . . B -2
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
Ho1 0.00990(11) 0.00824(11) 0.00883(9) -0.00071(10) -0.00180(10) 0.00063(10)
O1 0.0099(15) 0.0089(15) 0.0057(17) 0.0019(13) 0.0011(14) 0.0004(13)
O3 0.019(2) 0.018(2) 0.020(2) 0.0044(17) -0.0097(18) -0.0106(17)
O5 0.014(3) 0.009(2) 0.012(3) 0.000 0.000 -0.008(2)
O2L 0.019(2) 0.020(2) 0.018(2) -0.0008(18) -0.0068(18) 0.0060(18)
S1 0.0108(6) 0.0159(6) 0.0086(6) -0.0031(5) -0.0014(5) 0.0032(5)
O6 0.025(2) 0.0153(18) 0.016(2) -0.0033(16) -0.0056(18) 0.0094(17)
O7 0.0072(19) 0.037(3) 0.015(2) 0.0004(19) 0.0020(16) 0.0063(18)
C4 0.007(2) 0.012(2) 0.009(2) -0.0020(19) 0.001(2) -0.0006(19)
C0AA 0.017(3) 0.020(3) 0.008(2) -0.001(2) 0.002(2) -0.006(2)
C2AA 0.010(2) 0.013(2) 0.009(2) -0.002(2) -0.001(2) -0.0054(19)
C7 0.013(2) 0.015(3) 0.016(3) 0.002(2) -0.007(2) -0.004(2)
C6 0.016(2) 0.009(2) 0.018(3) 0.001(2) -0.001(3) -0.0035(19)
C5 0.009(2) 0.014(2) 0.008(2) -0.001(2) 0.002(2) -0.005(2)
C3 0.016(3) 0.013(2) 0.009(2) -0.001(2) -0.001(2) 0.001(2)
O2 0.0153(19) 0.0132(18) 0.0182(19) 0.0007(16) -0.0010(17) -0.0077(16)
O1L 0.021(2) 0.017(2) 0.026(2) 0.007(2) -0.004(2) 0.0042(18)
O1W 0.041(3) 0.029(3) 0.082(4) -0.006(3) 0.031(3) 0.001(3)
O4 0.0118(17) 0.0157(18) 0.0084(17) -0.0041(15) -0.0001(15) -0.0015(15)
C1AA 0.048(5) 0.048(5) 0.050(5) -0.001(3) 0.000(3) 0.000(3)
C9 0.026(9) 0.049(11) 0.047(6) -0.004(6) -0.010(5) 0.009(10)
N10 0.031(9) 0.046(11) 0.063(8) -0.015(8) 0.003(7) -0.006(8)
_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
Ho1 O1 2.353(3) . y
Ho1 O1 2.435(3) 4_655 y
Ho1 O1 2.380(3) 7_545 y
Ho1 O3 2.319(4) 6 y
Ho1 O2L 2.471(4) . y
Ho1 O2 2.315(4) . y
Ho1 O1L 2.405(4) . y
Ho1 O4 2.362(4) 3_646 y
O1 H1 0.9800 . ?
O3 C0AA 1.261(6) . ?
O5 C5 1.365(5) . ?
O5 C5 1.365(5) 4_765 ?
O2L H2LA 0.82(2) . ?
O2L H2LB 0.85(2) . ?
S1 O6 1.452(4) . ?
S1 O7 1.451(4) . ?
S1 C4 1.775(5) . ?
S1 O4 1.455(4) . ?
C4 C5 1.390(7) . ?
C4 C3 1.380(7) . ?
C0AA C2AA 1.495(7) . ?
C0AA O2 1.259(6) . ?
C2AA C7 1.374(7) . ?
C2AA C3 1.394(7) . ?
C7 H7 0.9300 . ?
C7 C6 1.390(7) . ?
C6 H6 0.9300 . ?
C6 C5 1.372(7) . ?
C3 H3 0.9300 . ?
O1L H1LA 0.82(2) . ?
O1L H1LB 0.82(2) . ?
O1W H 0.8451 . ?
O1W HA 0.8452 . ?
C1AA HB 0.9600 . ?
C1AA HC 0.9600 . ?
C1AA HD 0.9600 . ?
C1AA C9 1.459(12) . ?
C9 N10 1.25(2) . ?
O0AA HE 0.8447 . ?
O0AA HF 0.8445 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ho1 O1 72.47(13) . 7_545 y
O1 Ho1 O1 71.04(12) 7_545 4_655 y
O1 Ho1 O1 66.92(12) . 4_655 y
O1 Ho1 O2L 138.94(12) 4_655 . y
O1 Ho1 O2L 149.76(12) . . y
O1 Ho1 O2L 124.64(12) 7_545 . y
O1 Ho1 O1L 76.90(13) . . y
O1 Ho1 O1L 131.74(13) 7_545 . y
O1 Ho1 O4 105.57(12) . 3_646 y
O3 Ho1 O1 144.76(12) 6 4_655 y
O3 Ho1 O1 99.36(12) 6 . y
O3 Ho1 O1 73.89(12) 6 7_545 y
O3 Ho1 O2L 67.22(13) 6 . y
O3 Ho1 O1L 75.41(14) 6 . y
O3 Ho1 O4 137.86(13) 6 3_646 y
O2 Ho1 O1 79.50(12) . 4_655 y
O2 Ho1 O1 143.00(12) . . y
O2 Ho1 O1 82.55(12) . 7_545 y
O2 Ho1 O3 99.36(13) . 6 y
O2 Ho1 O2L 67.24(13) . . y
O2 Ho1 O1L 138.96(14) . . y
O2 Ho1 O4 80.45(13) . 3_646 y
O1L Ho1 O1 127.71(13) . 4_655 y
O1L Ho1 O2L 73.53(14) . . y
O4 Ho1 O1 146.07(11) 3_646 7_545 y
O4 Ho1 O1 77.10(11) 3_646 4_655 y
O4 Ho1 O2L 74.32(13) 3_646 . y
O4 Ho1 O1L 77.84(14) 3_646 . y
Ho1 O1 Ho1 102.33(12) 6 4_655 ?
Ho1 O1 Ho1 112.21(12) . 4_655 ?
Ho1 O1 Ho1 104.84(12) . 6 ?
Ho1 O1 H1 112.3 6 . ?
Ho1 O1 H1 112.3 4_655 . ?
Ho1 O1 H1 112.3 . . ?
C0AA O3 Ho1 127.2(3) . 7_545 ?
C5 O5 C5 118.5(6) 4_765 . ?
Ho1 O2L H2LA 120(3) . . ?
Ho1 O2L H2LB 117(3) . . ?
H2LA O2L H2LB 104(5) . . ?
O6 S1 C4 105.5(2) . . ?
O6 S1 O4 112.6(2) . . ?
O7 S1 O6 112.8(2) . . ?
O7 S1 C4 107.4(2) . . ?
O7 S1 O4 111.1(2) . . ?
O4 S1 C4 107.0(2) . . ?
C5 C4 S1 119.3(4) . . ?
C3 C4 S1 121.6(4) . . ?
C3 C4 C5 119.2(5) . . ?
O3 C0AA C2AA 117.0(5) . . ?
O2 C0AA O3 124.7(5) . . ?
O2 C0AA C2AA 118.3(5) . . ?
C7 C2AA C0AA 119.2(5) . . ?
C7 C2AA C3 119.2(5) . . ?
C3 C2AA C0AA 121.4(5) . . ?
C2AA C7 H7 119.4 . . ?
C2AA C7 C6 121.1(5) . . ?
C6 C7 H7 119.4 . . ?
C7 C6 H6 120.6 . . ?
C5 C6 C7 118.8(5) . . ?
C5 C6 H6 120.6 . . ?
O5 C5 C4 117.7(4) . . ?
O5 C5 C6 120.9(4) . . ?
C6 C5 C4 121.2(4) . . ?
C4 C3 C2AA 120.4(5) . . ?
C4 C3 H3 119.8 . . ?
C2AA C3 H3 119.8 . . ?
C0AA O2 Ho1 136.0(3) . . ?
Ho1 O1L H1LA 120(3) . . ?
Ho1 O1L H1LB 121(3) . . ?
H1LA O1L H1LB 115(5) . . ?
H O1W HA 104.3 . . ?
S1 O4 Ho1 146.0(2) . 2_666 ?
HB C1AA HC 109.5 . . ?
HB C1AA HD 109.5 . . ?
HC C1AA HD 109.5 . . ?
C9 C1AA HB 109.5 . . ?
C9 C1AA HC 109.5 . . ?
C9 C1AA HD 109.5 . . ?
N10 C9 C1AA 148(3) . . ?
HE O0AA HF 104.4 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O1W 0.98 2.14 3.093(6) 162.5 . yes
O1L H1LB O1W 0.82(2) 1.88(3) 2.681(7) 166(6) . yes
O1W HA N10 0.85 1.98 2.78(2) 158.4 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O3 C0AA C2AA 173.8(3) 7_545 . . . ?
Ho1 O3 C0AA O2 -6.1(8) 7_545 . . . ?
O3 C0AA C2AA C7 -4.6(7) . . . . ?
O3 C0AA C2AA C3 171.6(5) . . . . ?
O3 C0AA O2 Ho1 -39.6(8) . . . . ?
S1 C4 C5 O5 -8.2(6) . . . . ?
S1 C4 C5 C6 176.9(4) . . . . ?
S1 C4 C3 C2AA -178.8(4) . . . . ?
O6 S1 C4 C5 175.2(4) . . . . ?
O6 S1 C4 C3 -5.2(5) . . . . ?
O6 S1 O4 Ho1 -31.4(5) . . . 2_666 ?
O7 S1 C4 C5 -64.3(4) . . . . ?
O7 S1 C4 C3 115.3(4) . . . . ?
O7 S1 O4 Ho1 -159.0(4) . . . 2_666 ?
C4 S1 O4 Ho1 84.0(4) . . . 2_666 ?
C0AA C2AA C7 C6 174.8(5) . . . . ?
C0AA C2AA C3 C4 -174.9(5) . . . . ?
C2AA C0AA O2 Ho1 140.5(4) . . . . ?
C2AA C7 C6 C5 -0.3(8) . . . . ?
C7 C2AA C3 C4 1.3(8) . . . . ?
C7 C6 C5 O5 -172.2(5) . . . . ?
C7 C6 C5 C4 2.5(8) . . . . ?
C5 O5 C5 C4 124.7(5) 4_765 . . . ?
C5 O5 C5 C6 -60.4(4) 4_765 . . . ?
C5 C4 C3 C2AA 0.8(8) . . . . ?
C3 C4 C5 O5 172.2(4) . . . . ?
C3 C4 C5 C6 -2.7(7) . . . . ?
C3 C2AA C7 C6 -1.6(8) . . . . ?
O2 C0AA C2AA C7 175.3(5) . . . . ?
O2 C0AA C2AA C3 -8.5(7) . . . . ?
O4 S1 C4 C5 55.1(4) . . . . ?
O4 S1 C4 C3 -125.3(4) . . . . ?
loop_
_smtbx_masks_void_content
''
_shelx_res_file
;
TITL SBT1 in I-4
sb_154_0m.res
created by SHELXL-2017/1 at 10:26:07 on 23-Jan-2018
CELL 0.71073 12.8759 12.8759 16.2369 90 90 90
ZERR 2 0.0006 0.0006 0.0007 0 0 0
LATT -2
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SYMM -X,-Y,+Z
SFAC C H Ho N O S
UNIT 61.6 90.8 8 2.8 77.2 8
DFIX 0.85 O2L H2La O2L H2Lb
DFIX 0.85 O1L H1La O1L H1Lb
DFIX 1.456 0.01 C9 C1AA
DFIX 2.593 N10 C1AA
SADI Ho1 H2La Ho1 H2Lb
SADI Ho1 H1La Ho1 H1Lb
DANG 1.34 H2La H2Lb
DANG 1.34 H1La H1Lb
SIMU C1AA C9 N10
RIGU C1AA C9 N10
RIGU 0.001 0.001 N10 C1AA C9
ISOR 0.001 0.002 C1AA
L.S. 20
PLAN 20
TEMP 23
HTAB O1 O1W
HTAB O1L O1W
HTAB O1W N10
CONN 8 Ho1
BOND $H
CONF
fmap 2
acta
MERG 2
OMIT -3 60
REM
REM
REM >
REM
REM >
REM >
REM
REM
WGHT 0.007300
EXTI 0.000238
FVAR 0.22569
HO1 3 0.651047 -0.031689 0.326514 11.00000 0.00990 0.00824 =
0.00883 -0.00071 -0.00180 0.00063
O1 5 0.482720 -0.101078 0.314168 11.00000 0.00988 0.00894 =
0.00573 0.00186 0.00106 0.00040
AFIX 13
H1 2 0.471082 -0.159446 0.351789 11.00000 -1.20000
AFIX 0
O3 5 0.658583 0.243325 0.243571 11.00000 0.01927 0.01782 =
0.01968 0.00442 -0.00966 -0.01064
O5 5 1.000000 0.500000 0.427693 10.50000 0.01415 0.00917 =
0.01202 0.00000 0.00000 -0.00761
O2L 5 0.832125 -0.048167 0.375149 11.00000 0.01896 0.01969 =
0.01795 -0.00078 -0.00681 0.00600
H2LA 2 0.857445 -0.105559 0.382698 11.00000 -1.50000
H2LB 2 0.847988 -0.014463 0.418573 11.00000 -1.50000
S1 6 1.062898 0.287792 0.466525 11.00000 0.01083 0.01593 =
0.00855 -0.00313 -0.00143 0.00316
O6 5 1.052737 0.176298 0.477182 11.00000 0.02537 0.01528 =
0.01603 -0.00331 -0.00560 0.00939
O7 5 1.158551 0.316897 0.425311 11.00000 0.00721 0.03667 =
0.01467 0.00045 0.00197 0.00632
C4 1 0.958413 0.324749 0.401506 11.00000 0.00742 0.01162 =
0.00886 -0.00203 0.00055 -0.00059
C0AA 1 0.735585 0.206800 0.281869 11.00000 0.01656 0.01977 =
0.00778 -0.00070 0.00245 -0.00560
C2AA 1 0.812735 0.283047 0.314771 11.00000 0.00968 0.01279 =
0.00920 -0.00235 -0.00117 -0.00542
C7 1 0.800741 0.386707 0.297114 11.00000 0.01312 0.01540 =
0.01641 0.00190 -0.00689 -0.00388
AFIX 43
H7 2 0.748283 0.407484 0.261356 11.00000 -1.20000
AFIX 0
C6 1 0.865655 0.461060 0.331770 11.00000 0.01647 0.00880 =
0.01800 0.00133 -0.00086 -0.00349
AFIX 43
H6 2 0.857209 0.531041 0.319274 11.00000 -1.20000
AFIX 0
C5 1 0.942389 0.429424 0.384722 11.00000 0.00894 0.01352 =
0.00802 -0.00084 0.00248 -0.00536
C3 1 0.893025 0.251997 0.366785 11.00000 0.01588 0.01324 =
0.00855 -0.00064 -0.00097 0.00117
AFIX 43
H3 2 0.902593 0.181858 0.378161 11.00000 -1.20000
AFIX 0
O2 5 0.751677 0.111546 0.293986 11.00000 0.01534 0.01323 =
0.01817 0.00073 -0.00096 -0.00772
O1L 5 0.654345 -0.177413 0.419148 11.00000 0.02144 0.01677 =
0.02639 0.00658 -0.00381 0.00415
H1LA 2 0.703036 -0.218848 0.417623 11.00000 -1.50000
H1LB 2 0.600555 -0.199861 0.439673 11.00000 -1.50000
AFIX 6
O1W 5 0.468148 -0.255294 0.459771 11.00000 0.04109 0.02852 =
0.08222 -0.00589 0.03062 0.00101
H 2 0.484200 -0.244350 0.509490 11.00000 -1.50000
HA 2 0.456037 -0.319754 0.457694 11.00000 -1.50000
AFIX 0
O4 5 1.050346 0.344489 0.543431 11.00000 0.01181 0.01569 =
0.00835 -0.00410 -0.00011 -0.00154
PART -1
C1AA 1 0.495109 -0.503126 0.266801 10.35000 0.04795 0.04766 =
0.04950 -0.00105 -0.00034 0.00023
AFIX 137
HB 2 0.545105 -0.449156 0.257205 10.35000 -1.50000
HC 2 0.435449 -0.491896 0.232477 10.35000 -1.50000
HD 2 0.525496 -0.569248 0.253931 10.35000 -1.50000
AFIX 0
C9 1 0.463619 -0.501724 0.353091 10.35000 0.02610 0.04854 =
0.04714 -0.00384 -0.00966 0.00939
N10 4 0.416977 -0.455454 0.409696 10.35000 0.03098 0.04644 =
0.06291 -0.01467 0.00282 -0.00609
PART 0
PART -2
O0AA 5 0.442208 -0.522985 0.421726 10.15000 0.05874
AFIX 3
HE 2 0.491928 -0.528815 0.388106 10.15000 -1.50000
HF 2 0.394568 -0.494115 0.394266 10.15000 -1.50000
AFIX 0
HKLF 4
REM SBT1 in I-4
REM R1 = 0.0201 for 3368 Fo > 4sig(Fo) and 0.0208 for all 3441 data
REM 216 parameters refined using 37 restraints
END
WGHT 0.0073 0.0000
REM Highest difference peak 0.749, deepest hole -0.595, 1-sigma level 0.112
Q1 1 0.4559 -0.5024 0.2479 11.00000 0.05 0.75
Q2 1 0.5884 -0.0319 0.2983 11.00000 0.05 0.56
Q3 1 0.6557 -0.0059 0.2765 11.00000 0.05 0.55
Q4 1 0.7068 -0.0391 0.3644 11.00000 0.05 0.54
Q5 1 0.9786 0.3351 0.3599 11.00000 0.05 0.52
Q6 1 0.4997 -0.5392 0.2869 11.00000 0.05 0.51
Q7 1 0.3944 -0.4434 0.4767 11.00000 0.05 0.45
Q8 1 0.6421 -0.0910 0.2863 11.00000 0.05 0.45
Q9 1 0.6518 -0.0328 0.3826 11.00000 0.05 0.45
Q10 1 0.5885 -0.0279 0.3600 11.00000 0.05 0.43
Q11 1 0.7638 0.3526 0.1811 11.00000 0.05 0.41
Q12 1 0.4711 -0.1272 0.2774 11.00000 0.05 0.40
Q13 1 0.7106 -0.0342 0.2854 11.00000 0.05 0.39
Q14 1 0.4631 -0.4441 0.3347 11.00000 0.05 0.39
Q15 1 1.1158 0.3362 0.4622 11.00000 0.05 0.39
Q16 1 0.5000 -0.5000 0.2099 10.50000 0.05 0.39
Q17 1 1.0751 0.3280 0.4969 11.00000 0.05 0.39
Q18 1 0.7864 0.2391 0.2973 11.00000 0.05 0.39
Q19 1 0.8297 0.4314 0.3440 11.00000 0.05 0.39
Q20 1 0.5022 -0.2768 0.5021 11.00000 0.05 0.37
;
_shelx_res_checksum 80100
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_CP_2
_database_code_depnum_ccdc_archive 'CCDC 1838575'
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-10-02 downloaded from the CCDC.
;
_audit_creation_date 2018-01-23
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5356)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H32 Dy4 O34 S4, 4.6(H2 O), 1.4(C2 H3 N1)'
_chemical_formula_sum 'C30.80 H45.40 Dy4 N1.40 O38.60 S4'
_chemical_formula_weight 1831.12
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Dy Dy -0.1892 4.4098 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system tetragonal
_space_group_IT_number 82
_space_group_name_H-M_alt 'I -4'
_space_group_name_Hall 'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-y, x, -z'
'-x, -y, z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
_cell_length_a 12.8964(4)
_cell_length_b 12.8964(4)
_cell_length_c 16.2519(6)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2703.0(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6681
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 33.288
_cell_measurement_theta_min 3.364
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 5.726
_exptl_absorpt_correction_T_max 0.7465
_exptl_absorpt_correction_T_min 0.5159
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0931 before and 0.0502 after correction. The Ratio of minimum to maximum transmission is 0.6911. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.250
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1754
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.21
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0208
_diffrn_reflns_av_unetI/netI 0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 8591
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.974
_diffrn_reflns_theta_min 2.506
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.754
_reflns_Friedel_fraction_full 0.872
_reflns_Friedel_fraction_max 0.805
_reflns_number_gt 3510
_reflns_number_total 3557
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.579
_refine_diff_density_min -0.440
_refine_diff_density_rms 0.093
_refine_ls_abs_structure_details
;
Flack x determined using 1470 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.008(6)
_refine_ls_extinction_coef 0.00071(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref 0.918
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 220
_refine_ls_number_reflns 3557
_refine_ls_number_restraints 37
_refine_ls_R_factor_all 0.0170
_refine_ls_R_factor_gt 0.0166
_refine_ls_restrained_S_all 0.914
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0338
_refine_ls_wR_factor_ref 0.0340
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
O2L-H2LA = O2L-H2LB
0.85 with sigma of 0.02
O1L-H1LA = O1L-H1LB
0.85 with sigma of 0.02
C9-C1
1.456 with sigma of 0.01
N10-C1
2.593 with sigma of 0.02
H2LA-H2LB
1.34 with sigma of 0.04
H1LA-H1LB
1.34 with sigma of 0.04
Dy1-H2LA \\sim Dy1-H2LB
with sigma of 0.02
Dy1-H1LA \\sim Dy1-H1LB
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C9 \\sim N10: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
C1, C9, N10
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
N10, C1, C9
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
Fixed Sof: C1(0.35) H1A(0.35) H1B(0.35) H1C(0.35) C9(0.35) N10(0.35)
O0AA(0.15) H0AA(0.15) H0AB(0.15)
6.a Riding coordinates:
O0AA(H0AA,H0AB)
6.b Free rotating group:
O1W(H1WA,H1WB)
6.c Aromatic/amide H refined with riding coordinates:
C7(H7), C6(H6), C3(H3)
6.d Idealised Me refined as rotating group:
C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy -0.65057(2) 0.03211(2) -0.32623(2) 0.00796(5) Uani 1 1 d D . . . .
O1 O -0.4831(2) 0.1010(2) -0.31391(15) 0.0107(5) Uani 1 1 d . . . . .
O3 O -0.6592(3) -0.2415(3) -0.24382(18) 0.0204(7) Uani 1 1 d . . . . .
O5 O -1.000000 -0.500000 -0.4284(2) 0.0148(9) Uani 1 2 d S T P . .
O2L O -0.8309(3) 0.0508(3) -0.37445(19) 0.0236(7) Uani 1 1 d D . . . .
H2LA H -0.848(4) 0.111(2) -0.389(3) 0.035 Uiso 1 1 d DR . . . .
H2LB H -0.845(4) 0.017(4) -0.418(3) 0.035 Uiso 1 1 d DR . . . .
S1 S -1.06270(8) -0.28739(8) -0.46773(5) 0.01330(19) Uani 1 1 d . . . . .
O6 O -1.0526(3) -0.1759(2) -0.47916(18) 0.0207(6) Uani 1 1 d . . . . .
O7 O -1.1582(3) -0.3162(3) -0.42643(18) 0.0225(8) Uani 1 1 d . . . . .
C4 C -0.9584(3) -0.3237(3) -0.4022(2) 0.0109(7) Uani 1 1 d . . . . .
C0AA C -0.7365(3) -0.2057(4) -0.2821(2) 0.0147(8) Uani 1 1 d . . . . .
C2AA C -0.8128(3) -0.2813(3) -0.3156(2) 0.0143(8) Uani 1 1 d . . . . .
C7 C -0.8006(4) -0.3867(4) -0.2968(2) 0.0155(8) Uani 1 1 d . . . . .
H7 H -0.748439 -0.407236 -0.260825 0.019 Uiso 1 1 calc R . . . .
C6 C -0.8656(3) -0.4608(3) -0.3314(3) 0.0170(8) Uani 1 1 d . . . . .
H6 H -0.857528 -0.530598 -0.318661 0.020 Uiso 1 1 calc R . . . .
C5 C -0.9425(3) -0.4289(3) -0.3853(2) 0.0126(8) Uani 1 1 d . . . . .
C3 C -0.8931(3) -0.2505(3) -0.3676(2) 0.0143(8) Uani 1 1 d . . . . .
H3 H -0.902793 -0.180523 -0.379163 0.017 Uiso 1 1 calc R . . . .
O2 O -0.7521(3) -0.1103(3) -0.29426(18) 0.0179(6) Uani 1 1 d . . . . .
O1L O -0.6531(3) 0.1774(3) -0.4188(2) 0.0238(8) Uani 1 1 d D . . . .
H1LA H -0.699(3) 0.227(3) -0.419(3) 0.036 Uiso 1 1 d DR . . . .
H1LB H -0.602(3) 0.205(4) -0.443(3) 0.036 Uiso 1 1 d DR . . . .
O1W O -0.4677(4) 0.2564(3) -0.4588(3) 0.0545(13) Uani 1 1 d . . . . .
H1WA H -0.444250 0.239057 -0.505442 0.082 Uiso 1 1 d G . . . .
H1WB H -0.454748 0.320577 -0.455352 0.082 Uiso 1 1 d G . . . .
O4 O -1.0503(2) -0.3451(2) -0.54456(15) 0.0137(6) Uani 1 1 d . . . . .
C1 C -0.491(3) 0.504(5) -0.2657(8) 0.058(5) Uani 0.35 1 d D U . A -1
H1A H -0.564407 0.497530 -0.258370 0.086 Uiso 0.35 1 calc GR . . A -1
H1B H -0.467901 0.568912 -0.243154 0.086 Uiso 0.35 1 calc GR . . A -1
H1C H -0.456390 0.448079 -0.237931 0.086 Uiso 0.35 1 calc GR . . A -1
C9 C -0.4663(14) 0.500(2) -0.3530(8) 0.050(4) Uani 0.35 1 d D U . A -1
N10 N -0.4164(16) 0.4571(17) -0.4089(11) 0.060(4) Uani 0.35 1 d D U . A -1
O0AA O -0.434(4) 0.529(4) -0.421(3) 0.077(12) Uiso 0.15 1 d . . . B -2
H0AA H -0.483462 0.534431 -0.387877 0.116 Uiso 0.15 1 d R . . B -2
H0AB H -0.386102 0.499731 -0.394037 0.116 Uiso 0.15 1 d R . . B -2
H1 H -0.467(4) 0.149(4) -0.342(3) 0.018(12) 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
Dy1 0.00930(9) 0.00794(9) 0.00664(7) -0.00069(6) -0.00180(6) 0.00073(8)
O1 0.0121(13) 0.0099(12) 0.0101(12) 0.0036(10) 0.0010(10) -0.0019(12)
O3 0.0196(16) 0.0195(16) 0.0222(14) 0.0060(12) -0.0104(13) -0.0084(15)
O5 0.020(2) 0.016(2) 0.0095(16) 0.000 0.000 -0.008(2)
O2L 0.0237(18) 0.0260(18) 0.0212(15) -0.0008(14) -0.0063(14) 0.0046(17)
S1 0.0115(4) 0.0197(5) 0.0087(4) -0.0038(3) -0.0015(3) 0.0041(4)
O6 0.0281(17) 0.0163(15) 0.0177(13) -0.0048(12) -0.0051(13) 0.0076(15)
O7 0.0119(16) 0.039(2) 0.0166(14) -0.0022(14) 0.0025(12) 0.0060(16)
C4 0.0084(17) 0.0134(18) 0.0108(14) -0.0035(13) 0.0002(14) -0.0018(16)
C0AA 0.017(2) 0.017(2) 0.0109(16) 0.0006(15) -0.0006(15) -0.0047(18)
C2AA 0.0149(18) 0.0148(18) 0.0131(17) 0.0005(15) 0.0001(14) -0.0072(17)
C7 0.016(2) 0.016(2) 0.0140(16) 0.0006(15) -0.0042(15) -0.0016(18)
C6 0.020(2) 0.0134(18) 0.0178(17) 0.0024(17) -0.0031(18) -0.0021(17)
C5 0.0136(19) 0.0133(19) 0.0109(15) -0.0008(14) 0.0031(14) -0.0053(17)
C3 0.017(2) 0.014(2) 0.0119(16) -0.0013(15) 0.0023(15) -0.0012(18)
O2 0.0185(16) 0.0156(15) 0.0195(13) -0.0013(12) -0.0013(12) -0.0061(14)
O1L 0.0251(19) 0.0183(17) 0.0280(16) 0.0079(14) -0.0024(15) 0.0016(16)
O1W 0.046(3) 0.029(2) 0.088(4) -0.005(2) 0.036(3) -0.001(2)
O4 0.0151(14) 0.0174(15) 0.0087(11) -0.0043(10) 0.0011(10) -0.0007(13)
C1 0.058(6) 0.056(5) 0.059(5) -0.001(3) 0.000(3) 0.001(3)
C9 0.035(8) 0.061(11) 0.055(5) -0.011(6) -0.012(5) -0.006(10)
N10 0.055(10) 0.051(10) 0.073(8) -0.018(8) 0.009(8) -0.021(9)
_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
Dy1 O1 2.344(3) . y
Dy1 O1 2.440(3) 4_455 y
Dy1 O1 2.374(2) 7_454 y
Dy1 O3 2.315(3) 6_444 y
Dy1 O2L 2.466(4) . y
Dy1 O2 2.314(3) . y
Dy1 O1L 2.403(3) . y
Dy1 O4 2.354(3) 3_464 y
O1 H1 0.80(5) . ?
O3 C0AA 1.262(5) . ?
O5 C5 1.371(4) . ?
O5 C5 1.371(4) 4_345 ?
O2L H2LA 0.84(2) . ?
O2L H2LB 0.85(2) . ?
S1 O6 1.455(3) . ?
S1 O7 1.451(3) . ?
S1 C4 1.779(4) . ?
S1 O4 1.463(3) . ?
C4 C5 1.400(6) . ?
C4 C3 1.384(6) . ?
C0AA C2AA 1.488(6) . ?
C0AA O2 1.262(5) . ?
C2AA C7 1.402(6) . ?
C2AA C3 1.394(6) . ?
C7 H7 0.9300 . ?
C7 C6 1.390(6) . ?
C6 H6 0.9300 . ?
C6 C5 1.385(6) . ?
C3 H3 0.9300 . ?
O1L H1LA 0.87(2) . ?
O1L H1LB 0.85(2) . ?
O1W H1WA 0.8460 . ?
O1W H1WB 0.8464 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C9 1.455(12) . ?
C9 N10 1.24(2) . ?
O0AA H0AA 0.8458 . ?
O0AA H0AB 0.8457 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O1 72.60(11) . 7_454 y
O1 Dy1 O1 70.92(11) 7_454 4_455 y
O1 Dy1 O1 66.97(12) . 4_455 y
O1 Dy1 O2L 139.52(11) 4_455 . y
O1 Dy1 O2L 149.23(11) . . y
O1 Dy1 O2L 124.55(10) 7_454 . y
O1 Dy1 O1L 76.72(11) . . y
O1 Dy1 O1L 131.94(11) 7_454 . y
O1 Dy1 O4 105.59(10) . 3_464 y
O3 Dy1 O1 144.63(9) 6_444 4_455 y
O3 Dy1 O1 99.01(11) 6_444 . y
O3 Dy1 O1 73.92(10) 6_444 7_454 y
O3 Dy1 O2L 67.01(11) 6_444 . y
O3 Dy1 O1L 75.45(12) 6_444 . y
O3 Dy1 O4 138.28(10) 6_444 3_464 y
O2 Dy1 O1 79.80(11) . 4_455 y
O2 Dy1 O1 143.39(11) . . y
O2 Dy1 O1 82.62(10) . 7_454 y
O2 Dy1 O3 99.50(12) . 6_444 y
O2 Dy1 O2L 67.38(12) . . y
O2 Dy1 O1L 138.74(12) . . y
O2 Dy1 O4 80.15(10) . 3_464 y
O1L Dy1 O1 127.53(11) . 4_455 y
O1L Dy1 O2L 73.29(12) . . y
O4 Dy1 O1 145.59(10) 3_464 7_454 y
O4 Dy1 O1 76.84(9) 3_464 4_455 y
O4 Dy1 O2L 74.83(11) 3_464 . y
O4 Dy1 O1L 78.07(11) 3_464 . y
Dy1 O1 Dy1 102.12(10) 6_444 4_455 ?
Dy1 O1 Dy1 112.17(12) . 4_455 ?
Dy1 O1 Dy1 105.07(10) . 6_444 ?
Dy1 O1 H1 108(3) 6_444 . ?
Dy1 O1 H1 108(4) 4_455 . ?
Dy1 O1 H1 119(4) . . ?
C0AA O3 Dy1 128.0(3) . 7_454 ?
C5 O5 C5 118.6(4) 4_345 . ?
Dy1 O2L H2LA 115(3) . . ?
Dy1 O2L H2LB 114(3) . . ?
H2LA O2L H2LB 101(4) . . ?
O6 S1 C4 105.59(18) . . ?
O6 S1 O4 112.59(18) . . ?
O7 S1 O6 112.8(2) . . ?
O7 S1 C4 107.30(18) . . ?
O7 S1 O4 110.95(19) . . ?
O4 S1 C4 107.12(18) . . ?
C5 C4 S1 118.9(3) . . ?
C3 C4 S1 121.6(3) . . ?
C3 C4 C5 119.5(4) . . ?
O3 C0AA C2AA 117.6(4) . . ?
O3 C0AA O2 124.0(4) . . ?
O2 C0AA C2AA 118.4(4) . . ?
C7 C2AA C0AA 118.7(4) . . ?
C3 C2AA C0AA 121.8(4) . . ?
C3 C2AA C7 119.4(4) . . ?
C2AA C7 H7 119.6 . . ?
C6 C7 C2AA 120.7(4) . . ?
C6 C7 H7 119.6 . . ?
C7 C6 H6 120.5 . . ?
C5 C6 C7 118.9(4) . . ?
C5 C6 H6 120.5 . . ?
O5 C5 C4 117.9(3) . . ?
O5 C5 C6 120.8(4) . . ?
C6 C5 C4 121.1(4) . . ?
C4 C3 C2AA 120.2(4) . . ?
C4 C3 H3 119.9 . . ?
C2AA C3 H3 119.9 . . ?
C0AA O2 Dy1 135.9(3) . . ?
Dy1 O1L H1LA 126(3) . . ?
Dy1 O1L H1LB 128(3) . . ?
H1LA O1L H1LB 102(4) . . ?
H1WA O1W H1WB 104.3 . . ?
S1 O4 Dy1 145.38(19) . 2_444 ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C9 C1 H1A 109.5 . . ?
C9 C1 H1B 109.5 . . ?
C9 C1 H1C 109.5 . . ?
N10 C9 C1 147(3) . . ?
H0AA O0AA H0AB 104.4 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2L H2LA O6 0.84(2) 2.12(4) 2.785(4) 136(4) 4_355 yes
O2L H2LB O6 0.85(2) 1.91(3) 2.729(5) 160(5) 3_464 yes
O1L H1LA O7 0.87(2) 2.18(3) 3.025(5) 165(5) 4_355 yes
O1L H1LB O1W 0.85(2) 1.87(3) 2.678(6) 159(5) . yes
O1W H1WA O7 0.85 2.25 2.984(6) 145.9 2_544 yes
O1W H1WB N10 0.85 1.98 2.79(2) 161.0 . yes
O1W H1WB O0AA 0.85 2.49 3.00(5) 120.2 2_454 yes
O1W H1WB O0AA 0.85 2.48 3.11(5) 131.8 4_465 yes
O1 H1 O1W 0.80(5) 2.35(5) 3.099(6) 156(4) . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O3 C0AA C2AA -174.4(3) 7_454 . . . ?
Dy1 O3 C0AA O2 6.4(6) 7_454 . . . ?
O3 C0AA C2AA C7 5.8(6) . . . . ?
O3 C0AA C2AA C3 -171.6(4) . . . . ?
O3 C0AA O2 Dy1 39.1(6) . . . . ?
S1 C4 C5 O5 8.1(5) . . . . ?
S1 C4 C5 C6 -176.8(3) . . . . ?
S1 C4 C3 C2AA 179.2(3) . . . . ?
O6 S1 C4 C5 -174.8(3) . . . . ?
O6 S1 C4 C3 5.3(4) . . . . ?
O6 S1 O4 Dy1 31.5(4) . . . 2_444 ?
O7 S1 C4 C5 64.6(4) . . . . ?
O7 S1 C4 C3 -115.3(3) . . . . ?
O7 S1 O4 Dy1 159.1(3) . . . 2_444 ?
C4 S1 O4 Dy1 -84.1(3) . . . 2_444 ?
C0AA C2AA C7 C6 -175.5(4) . . . . ?
C0AA C2AA C3 C4 175.6(4) . . . . ?
C2AA C0AA O2 Dy1 -140.1(3) . . . . ?
C2AA C7 C6 C5 0.3(6) . . . . ?
C7 C2AA C3 C4 -1.8(6) . . . . ?
C7 C6 C5 O5 172.1(4) . . . . ?
C7 C6 C5 C4 -2.9(6) . . . . ?
C5 O5 C5 C4 -125.0(4) 4_345 . . . ?
C5 O5 C5 C6 59.9(3) 4_345 . . . ?
C5 C4 C3 C2AA -0.7(6) . . . . ?
C3 C4 C5 O5 -172.0(3) . . . . ?
C3 C4 C5 C6 3.1(6) . . . . ?
C3 C2AA C7 C6 2.0(6) . . . . ?
O2 C0AA C2AA C7 -174.9(4) . . . . ?
O2 C0AA C2AA C3 7.7(6) . . . . ?
O4 S1 C4 C5 -54.6(3) . . . . ?
O4 S1 C4 C3 125.5(3) . . . . ?
loop_
_smtbx_masks_void_content
None
_shelx_res_file
;
TITL TR1 in I-4
sb_136_0m.res
created by SHELXL-2017/1 at 10:17:10 on 23-Jan-2018
CELL 0.71073 12.8964 12.8964 16.2519 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT -2
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SYMM -X,-Y,+Z
SFAC C H Dy N O S
UNIT 61.6 90.8 8 2.8 77.2 8
EQIV $1 -2-X,-Y,+Z
EQIV $2 -1-Y,1+X,-1-Z
EQIV $3 +Y,-1-X,-1-Z
EQIV $4 -1-X,1-Y,+Z
EQIV $5 -1+Y,-X,-1-Z
DFIX 0.85 O2L H2La O2L H2Lb
DFIX 0.85 O1L H1La O1L H1Lb
DFIX 1.456 0.01 C9 C1
DFIX 2.593 N10 C1
SADI Dy1 H2La Dy1 H2Lb
SADI Dy1 H1La Dy1 H1Lb
DANG 1.34 H2La H2Lb
DANG 1.34 H1La H1Lb
SIMU C1 C9 N10
RIGU C1 C9 N10
RIGU 0.001 0.001 N10 C1 C9
ISOR 0.001 0.002 C1
L.S. 20
PLAN 20
TEMP 23
HTAB O1 O1W
HTAB O2L O6_$1
HTAB O2L O6_$2
HTAB O1L O7_$1
HTAB O1L O1W
HTAB O1W O7_$3
HTAB O1W N10
HTAB O1W O0AA_$4
HTAB O0AA N10_$4
HTAB O1W O0AA_$5
CONN 8 Dy1
BOND $H
CONF
fmap 2
acta
MERG 2
OMIT -3 60
REM
REM
REM >
REM
REM >
REM >
REM
REM
WGHT 0.000000
EXTI 0.000707
FVAR 0.23299
DY1 3 -0.650572 0.032114 -0.326226 11.00000 0.00930 0.00794 =
0.00664 -0.00069 -0.00180 0.00073
O1 5 -0.483054 0.100977 -0.313914 11.00000 0.01210 0.00995 =
0.01008 0.00358 0.00096 -0.00187
O3 5 -0.659229 -0.241490 -0.243820 11.00000 0.01961 0.01949 =
0.02220 0.00605 -0.01040 -0.00839
O5 5 -1.000000 -0.500000 -0.428350 10.50000 0.01952 0.01556 =
0.00947 0.00000 0.00000 -0.00821
O2L 5 -0.830917 0.050774 -0.374453 11.00000 0.02374 0.02595 =
0.02116 -0.00082 -0.00632 0.00464
H2LA 2 -0.847981 0.110929 -0.388966 11.00000 -1.50000
H2LB 2 -0.844508 0.016997 -0.418347 11.00000 -1.50000
S1 6 -1.062705 -0.287394 -0.467729 11.00000 0.01150 0.01969 =
0.00871 -0.00375 -0.00154 0.00411
O6 5 -1.052618 -0.175948 -0.479164 11.00000 0.02810 0.01634 =
0.01769 -0.00484 -0.00513 0.00756
O7 5 -1.158160 -0.316207 -0.426430 11.00000 0.01186 0.03905 =
0.01663 -0.00222 0.00255 0.00601
C4 1 -0.958370 -0.323685 -0.402168 11.00000 0.00836 0.01340 =
0.01084 -0.00355 0.00022 -0.00182
C0AA 1 -0.736470 -0.205690 -0.282108 11.00000 0.01663 0.01657 =
0.01090 0.00058 -0.00059 -0.00468
C2AA 1 -0.812760 -0.281251 -0.315643 11.00000 0.01493 0.01478 =
0.01306 0.00047 0.00012 -0.00716
C7 1 -0.800572 -0.386674 -0.296839 11.00000 0.01637 0.01609 =
0.01402 0.00061 -0.00419 -0.00160
AFIX 43
H7 2 -0.748439 -0.407236 -0.260825 11.00000 -1.20000
AFIX 0
C6 1 -0.865568 -0.460770 -0.331447 11.00000 0.01962 0.01343 =
0.01783 0.00243 -0.00315 -0.00210
AFIX 43
H6 2 -0.857528 -0.530598 -0.318661 11.00000 -1.20000
AFIX 0
C5 1 -0.942483 -0.428942 -0.385269 11.00000 0.01361 0.01327 =
0.01088 -0.00078 0.00311 -0.00533
C3 1 -0.893073 -0.250488 -0.367642 11.00000 0.01708 0.01391 =
0.01187 -0.00133 0.00234 -0.00117
AFIX 43
H3 2 -0.902793 -0.180523 -0.379163 11.00000 -1.20000
AFIX 0
O2 5 -0.752069 -0.110268 -0.294256 11.00000 0.01852 0.01560 =
0.01945 -0.00129 -0.00129 -0.00612
O1L 5 -0.653053 0.177395 -0.418757 11.00000 0.02506 0.01831 =
0.02804 0.00790 -0.00238 0.00160
H1LA 2 -0.698574 0.226720 -0.419398 11.00000 -1.50000
H1LB 2 -0.601677 0.204883 -0.443419 11.00000 -1.50000
AFIX 6
O1W 5 -0.467745 0.256396 -0.458830 11.00000 0.04604 0.02926 =
0.08825 -0.00492 0.03628 -0.00098
H1WA 2 -0.444250 0.239057 -0.505442 11.00000 -1.50000
H1WB 2 -0.454748 0.320577 -0.455352 11.00000 -1.50000
AFIX 0
O4 5 -1.050271 -0.345136 -0.544556 11.00000 0.01505 0.01745 =
0.00874 -0.00435 0.00105 -0.00073
PART -1
C1 1 -0.490829 0.504037 -0.265692 10.35000 0.05753 0.05648 =
0.05890 -0.00111 -0.00034 0.00102
AFIX 137
H1A 2 -0.564407 0.497530 -0.258370 10.35000 -1.50000
H1B 2 -0.467901 0.568912 -0.243154 10.35000 -1.50000
H1C 2 -0.456390 0.448079 -0.237931 10.35000 -1.50000
AFIX 0
C9 1 -0.466257 0.500382 -0.353035 10.35000 0.03456 0.06095 =
0.05550 -0.01062 -0.01182 -0.00579
N10 4 -0.416381 0.457107 -0.408917 10.35000 0.05538 0.05113 =
0.07340 -0.01818 0.00851 -0.02055
PART 0
PART -2
O0AA 5 -0.433742 0.528601 -0.421497 10.15000 0.07743
AFIX 3
H0AA 2 -0.483462 0.534431 -0.387877 10.15000 -1.50000
H0AB 2 -0.386102 0.499731 -0.394037 10.15000 -1.50000
AFIX 0
PART 0
H1 2 -0.466539 0.149208 -0.341873 11.00000 0.01814
HKLF 4
REM TR1 in I-4
REM R1 = 0.0166 for 3510 Fo > 4sig(Fo) and 0.0170 for all 3557 data
REM 220 parameters refined using 37 restraints
END
WGHT 0.0000 0.0000
REM Highest difference peak 0.579, deepest hole -0.440, 1-sigma level 0.093
Q1 1 -0.6386 0.0873 -0.3080 11.00000 0.05 0.58
Q2 1 -0.5966 0.0197 -0.3516 11.00000 0.05 0.53
Q3 1 -0.7018 0.0447 -0.3530 11.00000 0.05 0.52
Q4 1 -0.5947 0.0222 -0.3014 11.00000 0.05 0.49
Q5 1 -0.5392 0.5012 -0.2414 11.00000 0.05 0.47
Q6 1 -0.7025 0.0431 -0.3056 11.00000 0.05 0.46
Q7 1 -0.4858 0.5304 -0.2783 11.00000 0.05 0.46
Q8 1 -0.8935 -0.6067 -0.3262 11.00000 0.05 0.45
Q9 1 -0.6614 -0.0253 -0.3532 11.00000 0.05 0.45
Q10 1 -0.4834 0.2615 -0.5131 11.00000 0.05 0.43
Q11 1 -0.8603 -0.2875 -0.3466 11.00000 0.05 0.40
Q12 1 -0.6438 0.0228 -0.2679 11.00000 0.05 0.39
Q13 1 -0.9658 -0.3636 -0.3718 11.00000 0.05 0.35
Q14 1 -0.7762 -0.2498 -0.2994 11.00000 0.05 0.35
Q15 1 -0.8220 -0.3088 -0.2776 11.00000 0.05 0.35
Q16 1 -0.7994 -0.3351 -0.3201 11.00000 0.05 0.34
Q17 1 -0.9233 -0.1356 -0.3132 11.00000 0.05 0.33
Q18 1 -1.1592 -0.3797 -0.4746 11.00000 0.05 0.32
Q19 1 -0.6586 0.0331 -0.3859 11.00000 0.05 0.31
Q20 1 -0.3647 0.1978 -0.4977 11.00000 0.05 0.31
;
_shelx_res_checksum 28097
_olex2_submission_special_instructions 'No special instructions were received'