# 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
# this file and to allow appropriate attribution of the data.
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data_exp_17643
_database_code_depnum_ccdc_archive 'CCDC 1814436'
_audit_update_record
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_audit_creation_date 2018-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C19 H24 Mo3 N10 O9 S'
_chemical_formula_sum 'C19 H24 Mo3 N10 O9 S'
_chemical_formula_weight 856.36
_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'
Mo Mo -1.6832 0.6857 '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 triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.6290(3)
_cell_length_b 12.1305(4)
_cell_length_c 17.0785(6)
_cell_angle_alpha 109.173(3)
_cell_angle_beta 104.625(3)
_cell_angle_gamma 90.077(3)
_cell_volume 1626.85(10)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6830
_cell_measurement_temperature 173
_cell_measurement_theta_max 28.6780
_cell_measurement_theta_min 2.5020
_shelx_estimated_absorpt_T_max 0.951
_shelx_estimated_absorpt_T_min 0.704
_exptl_absorpt_coefficient_mu 1.261
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.91791
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour violet
_exptl_crystal_colour_primary violet
_exptl_crystal_density_diffrn 1.748
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 844
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.04
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0413
_diffrn_reflns_av_unetI/netI 0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 25698
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.916
_diffrn_reflns_theta_min 2.449
_diffrn_ambient_temperature 173
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -59.00 10.00 1.00 22.50 -- -22.85 -77.00 -90.00 69
2 \w -91.00 31.00 1.00 22.50 -- -22.85 -19.00 150.00 122
3 \w -93.00 -65.00 1.00 22.50 -- -22.85 -57.00 150.00 28
4 \w -47.00 -1.00 1.00 22.50 -- -22.85 -57.00 150.00 46
5 \w -55.00 40.00 1.00 22.50 -- -22.85 77.00-150.00 95
6 \w -47.00 40.00 1.00 22.50 -- -22.85 57.00 -30.00 87
7 \w -51.00 50.00 1.00 22.50 -- -22.85 77.00 120.00 101
8 \w -92.00 10.00 1.00 22.50 -- -22.85 -77.00 90.00 102
9 \w -77.00 -2.00 1.00 22.50 -- -22.85 -57.00 -30.00 75
10 \w -4.00 69.00 1.00 22.50 -- 24.10 -99.00 60.00 73
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0564673000
_diffrn_orient_matrix_UB_12 0.0500537000
_diffrn_orient_matrix_UB_13 0.0164092000
_diffrn_orient_matrix_UB_21 -0.0550534000
_diffrn_orient_matrix_UB_22 0.0289608000
_diffrn_orient_matrix_UB_23 -0.0232158000
_diffrn_orient_matrix_UB_31 -0.0325448000
_diffrn_orient_matrix_UB_32 0.0228268000
_diffrn_orient_matrix_UB_33 0.0357004000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6895
_reflns_number_total 8418
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 27.42
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_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 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 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 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.999
_refine_diff_density_min -0.843
_refine_diff_density_rms 0.115
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 406
_refine_ls_number_reflns 8418
_refine_ls_number_restraints 181
_refine_ls_R_factor_all 0.0508
_refine_ls_R_factor_gt 0.0388
_refine_ls_restrained_S_all 1.043
_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^)+(0.0396P)^2^+0.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0855
_refine_ls_wR_factor_ref 0.0913
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
N8-H8
0.88 with sigma of 0.01
N4-H4
0.88 with sigma of 0.01
N1-C5 \\sim N1-C5A
with sigma of 0.02
C4-C5 \\sim C4-C5A
with sigma of 0.02
N2-C4 \\sim N2-C4A
with sigma of 0.02
C4-C5 \\sim C4A-C5
with sigma of 0.02
C4-C5A \\sim C4A-C5A
with sigma of 0.02
C4A-C5A \\sim C4-C5
with sigma of 0.01
3. Rigid bond restraints
O5, C2, O7, C6, N1, N3, C10, N6, C12, N9, C19, N10, C18, C4, N2, N2, C3
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O3 \\sim O2 \\sim O1 \\sim O4 \\sim O5 \\sim O8 \\sim O7 \\sim O6 \\sim O9:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.01
C4 \\sim C4A \\sim C5 \\sim C5A: within 3.8A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.01
5. Others
Sof(H2B)=Sof(C4A)=Sof(H4AA)=1-FVAR(1)
Sof(H2A)=Sof(C4)=Sof(H4A)=FVAR(1)
Fixed Sof: C5(0.7) H5(0.7) C5A(0.3) H5A(0.3)
6.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
N2(H2A), N2(H2B), N6(H6), N10(H10), C14(H14), C12(H12), C8(H8A), C17(H17),
C3(H3), C4(H4A), C11(H11), C13(H13), C16(H16), C15(H15), C9(H9), C19(H19),
C10(H10A), C18(H18), C5(H5), C5A(H5A), C4A(H4AA)
;
_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
Mo2 Mo 0.41419(3) 0.74136(3) 0.73278(2) 0.02074(8) Uani 1 1 d . . . . .
Mo1 Mo 0.64628(3) 0.68534(3) 0.84186(2) 0.02004(8) Uani 1 1 d . . . . .
Mo3 Mo 0.42288(3) 0.52614(2) 0.73199(2) 0.01988(8) Uani 1 1 d . . . . .
S1 S 0.37762(10) 0.68524(7) 0.84726(5) 0.02138(17) Uani 1 1 d . . . . .
O3 O 0.6530(3) 0.5341(2) 0.75902(14) 0.0222(5) Uani 1 1 d . U . . .
O2 O 0.3975(3) 0.5929(2) 0.64214(14) 0.0234(5) Uani 1 1 d . U . . .
O1 O 0.6462(3) 0.7635(2) 0.75917(14) 0.0227(5) Uani 1 1 d . U . . .
O4 O 0.6998(3) 0.6344(2) 0.94396(14) 0.0269(5) Uani 1 1 d . U . . .
O5 O 0.9012(3) 0.6957(2) 0.87095(15) 0.0284(5) Uani 1 1 d . U . . .
O8 O 0.4100(3) 0.8217(2) 0.63862(15) 0.0306(6) Uani 1 1 d . U . . .
O7 O 0.3807(3) 0.9062(2) 0.79384(15) 0.0329(6) Uani 1 1 d . U . . .
N7 N 0.4417(3) 0.3643(3) 0.62912(17) 0.0250(6) Uani 1 1 d . . . . .
N9 N 0.1672(4) 0.4635(3) 0.69687(19) 0.0295(7) Uani 1 1 d . U . . .
N2 N 0.7008(4) 1.0118(3) 1.05676(19) 0.0323(7) Uani 1 1 d D U . . .
H2A H 0.7030 1.0498 1.1107 0.039 Uiso 0.34(8) 1 calc R . P A 1
H2B H 0.6812 1.0526 1.1058 0.039 Uiso 0.66(8) 1 calc R . P A 2
N1 N 0.6921(4) 0.8648(3) 0.93969(18) 0.0273(6) Uani 1 1 d D U . . .
N6 N 0.4343(4) 0.3682(3) 0.92874(19) 0.0332(7) Uani 1 1 d . U . . .
H6 H 0.4016 0.3614 0.9719 0.040 Uiso 1 1 calc R . . . .
N5 N 0.4452(3) 0.4189(3) 0.81796(18) 0.0254(6) Uani 1 1 d . . . . .
N8 N 0.5061(4) 0.2562(3) 0.5125(2) 0.0331(7) Uani 1 1 d D . . . .
N3 N 0.1447(4) 0.7272(3) 0.68233(19) 0.0324(7) Uani 1 1 d . U . . .
O6 O 1.1156(3) 0.6466(3) 0.9517(2) 0.0545(8) Uani 1 1 d . U . . .
N10 N -0.0853(4) 0.4505(3) 0.6981(2) 0.0435(9) Uani 1 1 d . U . . .
H10 H -0.1743 0.4667 0.7141 0.052 Uiso 1 1 calc R . . . .
C14 C 0.4947(4) 0.3644(3) 0.5619(2) 0.0284(8) Uani 1 1 d . . . . .
H14 H 0.5208 0.4331 0.5510 0.034 Uiso 1 1 calc R . . . .
C12 C 0.5633(5) 0.3203(4) 0.9023(3) 0.0389(9) Uani 1 1 d . U . . .
H12 H 0.6353 0.2742 0.9271 0.047 Uiso 1 1 calc R . . . .
N4 N -0.1107(4) 0.7328(4) 0.6781(2) 0.0470(10) Uani 1 1 d D . . . .
C8 C 0.0376(4) 0.7617(4) 0.7268(2) 0.0339(9) Uani 1 1 d . . . . .
H8A H 0.0649 0.8027 0.7870 0.041 Uiso 1 1 calc R . . . .
O9 O 0.3769(5) 0.9866(3) 0.6117(2) 0.0746(11) Uani 1 1 d . U . . .
C17 C 0.0573(4) 0.5058(3) 0.7389(2) 0.0312(8) Uani 1 1 d . . . . .
H17 H 0.0800 0.5687 0.7922 0.037 Uiso 1 1 calc R . . . .
C2 C 0.9710(4) 0.6561(4) 0.9309(2) 0.0338(8) Uani 1 1 d . U . . .
C3 C 0.6529(5) 0.8999(3) 1.0122(2) 0.0330(8) Uani 1 1 d . U . . .
H3 H 0.5962 0.8508 1.0310 0.040 Uiso 1 1 calc R . . . .
C4 C 0.746(4) 1.0556(11) 1.0006(13) 0.039(4) Uani 0.34(8) 1 d D U P A 1
H4A H 0.7695 1.1360 1.0095 0.047 Uiso 0.34(8) 1 calc R . P A 1
C11 C 0.3672(4) 0.4268(3) 0.8775(2) 0.0303(8) Uani 1 1 d . . . . .
H11 H 0.2754 0.4690 0.8826 0.036 Uiso 1 1 calc R . . . .
C13 C 0.5684(5) 0.3511(4) 0.8348(3) 0.0382(9) Uani 1 1 d . . . . .
H13 H 0.6459 0.3293 0.8030 0.046 Uiso 1 1 calc R . . . .
C1 C 0.8609(5) 0.6139(4) 0.9741(3) 0.0450(11) Uani 1 1 d . U . . .
H1A H 0.8676 0.5289 0.9630 0.054 Uiso 1 1 calc R . . . .
H1B H 0.8980 0.6548 1.0370 0.054 Uiso 1 1 calc R . . . .
C16 C 0.4218(6) 0.2485(4) 0.6206(3) 0.0464(11) Uani 1 1 d . . . . .
H16 H 0.3854 0.2194 0.6588 0.056 Uiso 1 1 calc R . . . .
C15 C 0.4627(6) 0.1811(4) 0.5481(3) 0.0476(11) Uani 1 1 d . . . . .
H15 H 0.4609 0.0981 0.5271 0.057 Uiso 1 1 calc R . . . .
C9 C -0.1026(6) 0.6661(6) 0.5976(3) 0.0692(16) Uani 1 1 d . U . . .
H9 H -0.1905 0.6285 0.5491 0.083 Uiso 1 1 calc R . . . .
C19 C 0.0837(5) 0.3697(4) 0.6261(3) 0.0592(14) Uani 1 1 d . U . . .
H19 H 0.1287 0.3181 0.5841 0.071 Uiso 1 1 calc R . . . .
C7 C 0.3827(6) 0.9300(4) 0.6590(3) 0.0454(11) Uani 1 1 d . . . . .
C10 C 0.0566(5) 0.6642(5) 0.6007(3) 0.0655(16) Uani 1 1 d . U . . .
H10A H 0.0994 0.6255 0.5537 0.079 Uiso 1 1 calc R . . . .
C18 C -0.0719(6) 0.3640(5) 0.6270(3) 0.0660(15) Uani 1 1 d . U . . .
H18 H -0.1563 0.3094 0.5853 0.079 Uiso 1 1 calc R . . . .
C6 C 0.3611(7) 0.9840(4) 0.7489(3) 0.0539(13) Uani 1 1 d . U . . .
H6A H 0.4401 1.0532 0.7813 0.065 Uiso 1 1 calc R . . . .
H6B H 0.2521 1.0112 0.7446 0.065 Uiso 1 1 calc R . . . .
H8 H 0.540(4) 0.233(3) 0.4655(15) 0.036(11) Uiso 1 1 d D . . . .
H4 H -0.208(3) 0.730(5) 0.685(3) 0.078(18) Uiso 1 1 d D . . . .
C5 C 0.7521(9) 0.9659(6) 0.9316(4) 0.039(2) Uani 0.7 1 d D U P A 1
H5 H 0.7904 0.9699 0.8851 0.047 Uiso 0.7 1 calc R . P A 1
C5A C 0.8056(19) 0.9542(11) 0.9545(11) 0.037(4) Uani 0.3 1 d D U P A 2
H5A H 0.8884 0.9466 0.9261 0.044 Uiso 0.3 1 calc R . P A 2
C4A C 0.785(4) 1.0523(9) 1.0134(13) 0.057(3) Uani 0.66(8) 1 d D U P A 2
H4AA H 0.8212 1.1309 1.0227 0.069 Uiso 0.66(8) 1 calc R . P A 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
Mo2 0.02385(15) 0.02310(15) 0.01969(14) 0.00754(12) 0.01314(12) 0.00686(11)
Mo1 0.02169(15) 0.02267(15) 0.01833(14) 0.00602(12) 0.01105(11) 0.00356(11)
Mo3 0.02212(15) 0.02140(15) 0.01865(14) 0.00526(12) 0.01191(11) 0.00413(11)
S1 0.0232(4) 0.0240(4) 0.0200(4) 0.0062(3) 0.0127(3) 0.0048(3)
O3 0.0244(12) 0.0235(12) 0.0208(11) 0.0051(10) 0.0125(9) 0.0056(9)
O2 0.0233(12) 0.0260(12) 0.0224(11) 0.0066(10) 0.0110(9) 0.0053(10)
O1 0.0261(12) 0.0233(12) 0.0219(11) 0.0059(10) 0.0144(9) 0.0036(9)
O4 0.0263(13) 0.0369(14) 0.0240(12) 0.0156(11) 0.0112(10) 0.0071(10)
O5 0.0247(12) 0.0367(14) 0.0276(12) 0.0118(11) 0.0123(10) 0.0034(10)
O8 0.0416(15) 0.0307(14) 0.0282(13) 0.0133(11) 0.0203(11) 0.0116(11)
O7 0.0512(16) 0.0256(13) 0.0307(13) 0.0104(10) 0.0252(12) 0.0153(11)
N7 0.0295(16) 0.0247(15) 0.0223(14) 0.0052(12) 0.0131(12) 0.0045(12)
N9 0.0302(15) 0.0313(16) 0.0285(15) 0.0057(12) 0.0165(12) 0.0028(12)
N2 0.0402(18) 0.0297(14) 0.0245(14) 0.0016(10) 0.0145(14) 0.0047(13)
N1 0.0335(17) 0.0246(15) 0.0245(13) 0.0041(11) 0.0146(13) 0.0010(13)
N6 0.0408(18) 0.0405(19) 0.0246(16) 0.0150(14) 0.0144(14) 0.0016(14)
N5 0.0277(16) 0.0269(16) 0.0247(15) 0.0080(13) 0.0132(12) 0.0051(12)
N8 0.0426(19) 0.0323(18) 0.0265(16) 0.0041(14) 0.0206(15) 0.0085(15)
N3 0.0269(16) 0.048(2) 0.0311(14) 0.0174(14) 0.0175(12) 0.0119(14)
O6 0.0280(16) 0.092(3) 0.0544(18) 0.0386(18) 0.0120(14) 0.0080(15)
N10 0.0299(18) 0.046(2) 0.048(2) 0.0027(15) 0.0183(15) -0.0001(15)
C14 0.0297(19) 0.029(2) 0.0267(18) 0.0055(16) 0.0135(15) 0.0029(15)
C12 0.039(2) 0.040(2) 0.047(2) 0.026(2) 0.0126(18) 0.0122(17)
N4 0.0271(19) 0.084(3) 0.038(2) 0.027(2) 0.0159(16) 0.0172(19)
C8 0.029(2) 0.044(2) 0.033(2) 0.0121(18) 0.0159(17) 0.0084(17)
O9 0.146(3) 0.0464(19) 0.060(2) 0.0343(17) 0.057(2) 0.032(2)
C17 0.029(2) 0.032(2) 0.034(2) 0.0075(17) 0.0147(16) 0.0020(16)
C2 0.025(2) 0.048(2) 0.0291(19) 0.0141(16) 0.0078(15) 0.0044(16)
C3 0.046(2) 0.0290(15) 0.0255(16) 0.0047(13) 0.0178(16) 0.0024(16)
C4 0.041(7) 0.036(4) 0.042(6) 0.012(5) 0.017(5) -0.002(5)
C11 0.032(2) 0.035(2) 0.0299(19) 0.0154(17) 0.0132(16) 0.0040(16)
C13 0.044(2) 0.042(2) 0.044(2) 0.024(2) 0.026(2) 0.0164(19)
C1 0.030(2) 0.071(3) 0.047(2) 0.036(2) 0.0093(18) 0.009(2)
C16 0.072(3) 0.034(2) 0.042(2) 0.012(2) 0.031(2) 0.004(2)
C15 0.077(3) 0.027(2) 0.043(2) 0.0075(19) 0.029(2) 0.010(2)
C9 0.039(3) 0.121(5) 0.041(3) 0.020(3) 0.007(2) 0.016(3)
C19 0.040(2) 0.066(3) 0.047(3) -0.0190(19) 0.0195(18) -0.004(2)
C7 0.079(3) 0.032(2) 0.044(2) 0.021(2) 0.037(2) 0.020(2)
C10 0.036(3) 0.124(5) 0.0286(18) 0.013(2) 0.0128(16) 0.019(3)
C18 0.0383(17) 0.072(3) 0.058(3) -0.019(2) 0.017(2) -0.011(2)
C6 0.100(4) 0.036(2) 0.046(2) 0.0218(18) 0.044(3) 0.024(2)
C5 0.051(5) 0.040(4) 0.026(4) 0.001(3) 0.023(3) -0.010(3)
C5A 0.041(9) 0.038(7) 0.033(8) 0.004(6) 0.022(7) -0.005(6)
C4A 0.069(8) 0.041(4) 0.053(5) -0.015(4) 0.042(6) -0.025(4)
_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
Mo2 Mo1 2.6257(4) . ?
Mo2 Mo3 2.6075(4) . ?
Mo2 S1 2.3604(8) . ?
Mo2 O2 1.927(2) . ?
Mo2 O1 1.936(2) . ?
Mo2 O8 2.130(2) . ?
Mo2 O7 1.988(2) . ?
Mo2 N3 2.251(3) . ?
Mo1 Mo3 2.5980(4) . ?
Mo1 S1 2.3433(8) . ?
Mo1 O3 1.926(2) . ?
Mo1 O1 1.942(2) . ?
Mo1 O4 1.984(2) . ?
Mo1 O5 2.123(2) . ?
Mo1 N1 2.228(3) . ?
Mo3 S1 2.3764(8) . ?
Mo3 O3 1.916(2) . ?
Mo3 O2 1.925(2) . ?
Mo3 N7 2.201(3) . ?
Mo3 N9 2.198(3) . ?
Mo3 N5 2.236(3) . ?
O4 C1 1.408(4) . ?
O5 C2 1.286(4) . ?
O8 C7 1.283(5) . ?
O7 C6 1.386(5) . ?
N7 C14 1.339(4) . ?
N7 C16 1.370(5) . ?
N9 C17 1.335(4) . ?
N9 C19 1.389(5) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N2 C3 1.324(5) . ?
N2 C4 1.371(14) . ?
N2 C4A 1.354(9) . ?
N1 C3 1.302(4) . ?
N1 C5 1.391(7) . ?
N1 C5A 1.375(14) . ?
N6 H6 0.8800 . ?
N6 C12 1.365(5) . ?
N6 C11 1.327(5) . ?
N5 C11 1.334(4) . ?
N5 C13 1.376(5) . ?
N8 C14 1.326(5) . ?
N8 C15 1.348(5) . ?
N8 H8 0.881(10) . ?
N3 C8 1.324(4) . ?
N3 C10 1.368(5) . ?
O6 C2 1.225(4) . ?
N10 H10 0.8800 . ?
N10 C17 1.307(5) . ?
N10 C18 1.350(5) . ?
C14 H14 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.333(5) . ?
N4 C8 1.312(5) . ?
N4 C9 1.368(6) . ?
N4 H4 0.875(10) . ?
C8 H8A 0.9500 . ?
O9 C7 1.213(5) . ?
C17 H17 0.9500 . ?
C2 C1 1.519(5) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9500 . ?
C4 C5 1.328(9) . ?
C11 H11 0.9500 . ?
C13 H13 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C15 1.372(5) . ?
C15 H15 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.362(6) . ?
C19 H19 0.9500 . ?
C19 C18 1.348(6) . ?
C7 C6 1.517(5) . ?
C10 H10A 0.9500 . ?
C18 H18 0.9500 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C5 H5 0.9500 . ?
C5A H5A 0.9500 . ?
C5A C4A 1.327(9) . ?
C4A H4AA 0.9500 . ?
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
Mo3 Mo2 Mo1 59.527(11) . . ?
S1 Mo2 Mo1 55.76(2) . . ?
S1 Mo2 Mo3 56.89(2) . . ?
O2 Mo2 Mo1 93.83(7) . . ?
O2 Mo2 Mo3 47.37(7) . . ?
O2 Mo2 S1 102.68(7) . . ?
O2 Mo2 O1 94.05(9) . . ?
O2 Mo2 O8 87.04(9) . . ?
O2 Mo2 O7 160.62(10) . . ?
O2 Mo2 N3 84.23(11) . . ?
O1 Mo2 Mo1 47.49(7) . . ?
O1 Mo2 Mo3 91.86(7) . . ?
O1 Mo2 S1 102.07(7) . . ?
O1 Mo2 O8 86.16(10) . . ?
O1 Mo2 O7 96.86(10) . . ?
O1 Mo2 N3 169.64(10) . . ?
O8 Mo2 Mo1 133.62(7) . . ?
O8 Mo2 Mo3 134.16(7) . . ?
O8 Mo2 S1 166.63(7) . . ?
O8 Mo2 N3 83.56(10) . . ?
O7 Mo2 Mo1 105.35(8) . . ?
O7 Mo2 Mo3 147.53(7) . . ?
O7 Mo2 S1 90.67(7) . . ?
O7 Mo2 O8 77.79(9) . . ?
O7 Mo2 N3 82.17(12) . . ?
N3 Mo2 Mo1 142.73(8) . . ?
N3 Mo2 Mo3 94.42(9) . . ?
N3 Mo2 S1 88.26(8) . . ?
Mo3 Mo1 Mo2 59.889(11) . . ?
S1 Mo1 Mo2 56.38(2) . . ?
S1 Mo1 Mo3 57.21(2) . . ?
O3 Mo1 Mo2 92.57(7) . . ?
O3 Mo1 Mo3 47.30(7) . . ?
O3 Mo1 S1 103.36(7) . . ?
O3 Mo1 O1 92.02(9) . . ?
O3 Mo1 O4 96.04(10) . . ?
O3 Mo1 O5 85.30(9) . . ?
O3 Mo1 N1 168.24(10) . . ?
O1 Mo1 Mo2 47.29(7) . . ?
O1 Mo1 Mo3 92.01(7) . . ?
O1 Mo1 S1 102.48(7) . . ?
O1 Mo1 O4 164.48(10) . . ?
O1 Mo1 O5 88.59(9) . . ?
O1 Mo1 N1 85.56(10) . . ?
O4 Mo1 Mo2 144.93(7) . . ?
O4 Mo1 Mo3 103.20(7) . . ?
O4 Mo1 S1 88.55(7) . . ?
O4 Mo1 O5 78.92(9) . . ?
O4 Mo1 N1 83.85(11) . . ?
O5 Mo1 Mo2 135.78(7) . . ?
O5 Mo1 Mo3 132.59(7) . . ?
O5 Mo1 S1 165.54(7) . . ?
O5 Mo1 N1 83.14(10) . . ?
N1 Mo1 Mo2 94.21(8) . . ?
N1 Mo1 Mo3 144.18(8) . . ?
N1 Mo1 S1 88.40(8) . . ?
Mo1 Mo3 Mo2 60.584(11) . . ?
S1 Mo3 Mo2 56.31(2) . . ?
S1 Mo3 Mo1 55.99(2) . . ?
O3 Mo3 Mo2 93.36(7) . . ?
O3 Mo3 Mo1 47.60(7) . . ?
O3 Mo3 S1 102.46(7) . . ?
O3 Mo3 O2 95.40(9) . . ?
O3 Mo3 N7 82.61(10) . . ?
O3 Mo3 N9 163.37(11) . . ?
O3 Mo3 N5 85.58(10) . . ?
O2 Mo3 Mo2 47.44(7) . . ?
O2 Mo3 Mo1 94.75(7) . . ?
O2 Mo3 S1 102.17(7) . . ?
O2 Mo3 N7 83.04(10) . . ?
O2 Mo3 N9 94.34(10) . . ?
O2 Mo3 N5 170.12(10) . . ?
N7 Mo3 Mo2 129.87(7) . . ?
N7 Mo3 Mo1 129.89(8) . . ?
N7 Mo3 S1 172.22(8) . . ?
N7 Mo3 N5 87.35(10) . . ?
N9 Mo3 Mo2 103.16(8) . . ?
N9 Mo3 Mo1 144.55(8) . . ?
N9 Mo3 S1 88.59(8) . . ?
N9 Mo3 N7 85.23(11) . . ?
N9 Mo3 N5 82.55(11) . . ?
N5 Mo3 Mo2 142.40(7) . . ?
N5 Mo3 Mo1 93.15(8) . . ?
N5 Mo3 S1 87.17(7) . . ?
Mo2 S1 Mo3 66.80(2) . . ?
Mo1 S1 Mo2 67.87(2) . . ?
Mo1 S1 Mo3 66.79(2) . . ?
Mo3 O3 Mo1 85.10(9) . . ?
Mo3 O2 Mo2 85.19(9) . . ?
Mo2 O1 Mo1 85.22(9) . . ?
C1 O4 Mo1 117.0(2) . . ?
C2 O5 Mo1 115.3(2) . . ?
C7 O8 Mo2 116.5(2) . . ?
C6 O7 Mo2 118.3(2) . . ?
C14 N7 Mo3 122.9(2) . . ?
C14 N7 C16 105.0(3) . . ?
C16 N7 Mo3 131.8(2) . . ?
C17 N9 Mo3 128.1(2) . . ?
C17 N9 C19 104.2(3) . . ?
C19 N9 Mo3 127.7(2) . . ?
C3 N2 H2A 127.5 . . ?
C3 N2 H2B 126.1 . . ?
C3 N2 C4 105.1(7) . . ?
C3 N2 C4A 107.8(4) . . ?
C4 N2 H2A 127.5 . . ?
C4A N2 H2B 126.1 . . ?
C3 N1 Mo1 127.4(3) . . ?
C3 N1 C5 105.3(4) . . ?
C3 N1 C5A 100.2(7) . . ?
C5 N1 Mo1 126.9(3) . . ?
C5A N1 Mo1 129.6(6) . . ?
C12 N6 H6 126.2 . . ?
C11 N6 H6 126.2 . . ?
C11 N6 C12 107.5(3) . . ?
C11 N5 Mo3 127.8(2) . . ?
C11 N5 C13 104.6(3) . . ?
C13 N5 Mo3 126.1(2) . . ?
C14 N8 C15 108.2(3) . . ?
C14 N8 H8 129(3) . . ?
C15 N8 H8 123(3) . . ?
C8 N3 Mo2 127.9(3) . . ?
C8 N3 C10 105.2(3) . . ?
C10 N3 Mo2 126.2(3) . . ?
C17 N10 H10 126.0 . . ?
C17 N10 C18 107.9(3) . . ?
C18 N10 H10 126.0 . . ?
N7 C14 H14 124.4 . . ?
N8 C14 N7 111.3(3) . . ?
N8 C14 H14 124.4 . . ?
N6 C12 H12 126.8 . . ?
C13 C12 N6 106.5(3) . . ?
C13 C12 H12 126.8 . . ?
C8 N4 C9 107.0(3) . . ?
C8 N4 H4 138(3) . . ?
C9 N4 H4 113(3) . . ?
N3 C8 H8A 123.8 . . ?
N4 C8 N3 112.3(3) . . ?
N4 C8 H8A 123.8 . . ?
N9 C17 H17 124.0 . . ?
N10 C17 N9 112.0(3) . . ?
N10 C17 H17 124.0 . . ?
O5 C2 C1 115.8(3) . . ?
O6 C2 O5 124.4(3) . . ?
O6 C2 C1 119.7(4) . . ?
N2 C3 H3 123.8 . . ?
N1 C3 N2 112.4(3) . . ?
N1 C3 H3 123.8 . . ?
N2 C4 H4A 126.0 . . ?
C5 C4 N2 108.0(10) . . ?
C5 C4 H4A 126.0 . . ?
N6 C11 N5 111.2(3) . . ?
N6 C11 H11 124.4 . . ?
N5 C11 H11 124.4 . . ?
N5 C13 H13 124.9 . . ?
C12 C13 N5 110.2(3) . . ?
C12 C13 H13 124.9 . . ?
O4 C1 C2 112.0(3) . . ?
O4 C1 H1A 109.2 . . ?
O4 C1 H1B 109.2 . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N7 C16 H16 125.4 . . ?
N7 C16 C15 109.2(4) . . ?
C15 C16 H16 125.4 . . ?
N8 C15 C16 106.3(4) . . ?
N8 C15 H15 126.9 . . ?
C16 C15 H15 126.9 . . ?
N4 C9 H9 126.8 . . ?
C10 C9 N4 106.4(4) . . ?
C10 C9 H9 126.8 . . ?
N9 C19 H19 125.7 . . ?
C18 C19 N9 108.6(4) . . ?
C18 C19 H19 125.7 . . ?
O8 C7 C6 114.6(3) . . ?
O9 C7 O8 123.4(4) . . ?
O9 C7 C6 121.9(4) . . ?
N3 C10 H10A 125.6 . . ?
C9 C10 N3 108.9(4) . . ?
C9 C10 H10A 125.6 . . ?
N10 C18 H18 126.4 . . ?
C19 C18 N10 107.2(4) . . ?
C19 C18 H18 126.4 . . ?
O7 C6 C7 112.6(3) . . ?
O7 C6 H6A 109.1 . . ?
O7 C6 H6B 109.1 . . ?
C7 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
N1 C5 H5 126.1 . . ?
C4 C5 N1 107.8(9) . . ?
C4 C5 H5 126.1 . . ?
N1 C5A H5A 124.1 . . ?
C4A C5A N1 111.9(10) . . ?
C4A C5A H5A 124.1 . . ?
N2 C4A H4AA 128.9 . . ?
C5A C4A N2 102.1(10) . . ?
C5A C4A H4AA 128.9 . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 362.9 86.3 'H2O, C3H4N2'
_shelx_fab_file
;
-12 1 7 -1.8498 -0.0026
-11 -6 7 0.0405 0.0345
-11 -6 8 -1.1664 -0.0424
-11 -6 9 0.6598 0.0630
-11 -5 6 1.3172 -0.0368
-11 -5 7 0.0806 0.0271
-11 -5 8 -0.4740 -0.0125
-11 -5 9 0.9915 0.0171
-11 -4 1 -0.6738 -0.1092
-11 -4 2 0.4099 -0.0489
-11 -4 5 -0.8796 0.0158
-11 -4 6 1.4649 -0.0302
-11 -4 7 0.1070 0.0308
-11 -4 8 -1.2786 0.0071
-11 -4 9 0.8579 -0.0070
-11 -4 10 -0.0797 -0.0041
-11 -3 4 -1.1069 -0.0354
-11 -3 5 -1.6461 -0.0431
-11 -3 6 0.7618 -0.0427
-11 -3 7 1.5417 0.0368
-11 -3 8 -0.9881 0.0272
-11 -3 9 -0.3709 -0.0228
-11 -3 10 0.5340 0.0312
-11 -3 11 -0.9088 -0.0091
-11 -3 12 -1.2546 0.0039
-11 -2 3 1.6130 0.0302
-11 -2 4 -0.1031 -0.0034
-11 -2 5 -1.0480 -0.0203
-11 -2 6 -0.7093 -0.0354
-11 -2 7 0.9599 0.0100
-11 -2 8 0.9306 0.0019
-11 -2 9 -1.1298 -0.0647
-11 -2 10 -0.6825 0.0716
-11 -2 11 0.4288 -0.0049
-11 -2 12 0.1731 -0.0149
-11 -1 1 -0.9148 0.0545
-11 -1 2 0.1996 0.0319
-11 -1 3 0.9827 0.0057
-11 -1 4 -0.4496 -0.0491
-11 -1 5 0.0444 -0.0086
-11 -1 6 0.3929 -0.0017
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-11 -1 8 2.2570 -0.0103
-11 -1 9 0.2207 -0.0973
-11 -1 10 -0.9412 0.0652
-11 -1 11 -1.4342 0.0108
-11 -1 12 0.5005 0.0159
-11 -1 13 -1.1671 0.0225
-11 0 1 -0.6586 0.0105
-11 0 2 0.2397 0.0891
-11 0 3 1.3302 0.0413
-11 0 4 -1.0906 -0.0520
-11 0 5 -1.3122 -0.0007
-11 0 6 1.3027 -0.0107
-11 0 7 -1.1287 0.0492
-11 0 8 1.1521 -0.0019
-11 0 9 0.4699 -0.0836
-11 0 10 1.5485 0.0252
-11 0 11 -0.7024 -0.0334
-11 0 12 0.4290 0.0404
-11 0 13 -3.4879 0.0926
-11 1 1 -0.8629 -0.0499
-11 1 2 -0.6137 0.0466
-11 1 3 1.0592 0.0508
-11 1 4 0.0459 -0.0278
-11 1 5 -1.5887 0.0170
-11 1 6 -0.2375 -0.0172
-11 1 7 0.1083 0.0391
-11 1 8 0.5052 0.0198
-11 1 9 -0.6892 -0.0398
-11 1 10 0.8071 0.0174
-11 1 11 -0.4744 -0.0559
-11 1 12 2.2283 0.0049
-11 2 1 0.7031 -0.0166
-11 2 2 0.5871 -0.0531
-11 2 3 0.0240 -0.0090
-11 2 4 -0.2433 -0.0097
-11 2 5 0.0768 0.0335
-11 2 6 -1.7119 0.0093
-11 2 7 0.1010 -0.0062
-11 2 8 -0.2214 0.0174
-11 2 9 0.6472 -0.0166
-11 3 1 -0.4879 0.1304
-11 3 2 1.9302 0.0110
-11 3 3 1.5205 -0.0356
-11 3 4 -0.5554 -0.0500
-11 3 5 0.7689 -0.0212
-11 3 6 -0.8098 0.0362
-11 4 1 -1.8825 -0.0035
-11 4 2 -0.5803 0.0481
-11 4 3 1.3491 0.0526
-11 6 5 0.5684 0.1036
-10 -9 8 -0.3391 -0.2605
-10 -9 9 -0.5095 0.0190
-10 -8 4 6.8086 0.0396
-10 -8 5 -1.9821 0.0175
-10 -8 6 -2.3096 0.0923
-10 -8 7 -1.3031 0.0249
-10 -8 8 -0.0283 -0.0702
-10 -8 9 -0.7400 -0.0080
-10 -8 10 -0.0284 0.0241
-10 -8 11 0.5177 -0.0749
-10 -8 12 2.0348 0.0571
-10 -7 3 -1.8576 -0.0563
-10 -7 4 2.2664 -0.0143
-10 -7 5 2.9609 0.1046
-10 -7 6 0.1585 0.0444
-10 -7 7 -2.0400 -0.0274
-10 -7 8 -0.5645 0.0085
-10 -7 9 0.4461 0.0566
-10 -7 10 -0.7829 -0.0373
-10 -7 11 -0.5226 -0.1494
-10 -7 12 1.2468 0.0985
-10 -6 2 -0.4453 0.0073
-10 -6 3 0.9210 -0.0080
-10 -6 4 -2.3721 -0.0600
-10 -6 5 1.9913 0.0352
-10 -6 6 1.8966 0.0322
-10 -6 7 -0.7247 0.0114
-10 -6 8 -0.5223 0.0280
-10 -6 9 0.5394 0.0765
-10 -6 10 -0.3980 0.0115
-10 -6 11 -0.2611 -0.0779
-10 -6 12 0.0995 0.0177
-10 -6 13 0.9469 -0.0425
-10 -5 1 -0.2003 -0.1223
-10 -5 2 -0.9755 -0.0316
-10 -5 3 1.6931 -0.0135
-10 -5 4 -1.5752 0.0198
-10 -5 5 0.1998 -0.0224
-10 -5 6 0.9357 -0.0520
-10 -5 7 -0.8304 0.0022
-10 -5 8 0.5624 0.0370
-10 -5 9 0.7766 0.0311
-10 -5 10 -0.0887 -0.0116
-10 -5 11 0.1237 0.0324
-10 -5 12 0.0349 0.0603
-10 -5 13 -0.0558 -0.0252
-10 -5 14 0.3227 -0.0755
-10 -5 15 0.6254 0.0434
-10 -4 1 -0.0116 -0.0414
-10 -4 2 0.7064 -0.0150
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10 -4 0 -0.9886 0.0199
10 -4 1 0.3944 0.0350
10 -4 2 -0.5723 0.0351
10 -4 3 -1.1398 -0.0387
10 -4 4 -0.1258 -0.0671
10 -4 5 2.1920 -0.0073
10 -3 0 -1.9304 -0.0358
10 -3 1 0.0481 0.0276
10 -3 2 -0.0396 0.0169
10 -3 3 -1.2080 0.0638
10 -3 4 -1.2831 -0.0239
10 -3 5 1.6921 -0.0329
10 -2 0 -0.3205 0.0050
10 -2 1 0.5142 0.0220
10 -2 2 1.3732 -0.0248
10 -2 3 -0.6775 0.0191
10 -2 4 -1.0976 0.0159
10 -2 5 -0.3641 0.0086
10 -1 0 -1.2888 -0.0028
10 -1 1 -0.3689 0.0126
10 -1 2 2.1922 -0.0052
10 -1 3 -0.0224 -0.0048
10 -1 4 0.6577 0.0057
10 0 0 -1.4380 0.0076
10 0 1 -1.4184 0.0072
10 0 2 1.1905 -0.0170
10 0 3 0.3279 0.0093
10 0 4 -0.6989 -0.0556
10 0 5 0.3503 -0.0519
10 0 6 0.9471 0.0176
10 0 7 0.8594 0.1989
10 1 0 -0.3677 -0.0032
10 1 1 -0.7134 -0.0031
10 1 2 -0.8570 -0.0186
10 1 3 2.3374 0.0974
10 1 4 -0.3553 -0.0088
10 1 5 -1.3659 -0.0935
10 1 6 0.1144 -0.1475
10 2 0 -0.0962 0.0195
10 2 1 1.4695 -0.0283
10 2 2 -2.4689 -0.0422
10 2 3 0.6200 0.0968
10 2 4 0.3754 0.0464
10 2 5 0.4651 -0.0066
10 3 0 -1.4670 -0.0153
10 3 1 1.9270 -0.0485
10 3 2 0.5174 -0.0235
10 3 3 -0.7842 0.0434
10 3 4 -1.7718 0.0554
10 4 0 -1.0229 -0.0684
10 4 1 -0.8867 -0.0735
10 4 2 1.7957 -0.0008
10 5 0 0.5737 -0.0379
10 5 1 -1.0474 -0.0658
11 -4 0 0.0518 0.0971
11 -4 1 0.4734 0.0956
11 -4 2 -2.4235 0.0503
11 -4 3 1.4652 -0.0988
11 -3 0 -0.8893 -0.0486
11 -3 1 0.9060 0.0527
11 -3 2 -2.9630 0.0783
11 -2 0 0.3764 -0.0251
11 -2 1 2.1056 -0.0387
11 -1 0 -0.6570 0.0556
11 0 0 -1.2273 0.0482
11 3 0 0.2344 -0.1098
11 3 1 -0.6363 -0.0626
0 0 0 0.0 0.0
;
_iucr_refine_instructions_details
;
exp_17643.res created by SHELXL-2014/7
TITL exp_17643_a.res in P-1
REM Old TITL exp_17643 in P-1
REM SHELXT solution in P-1
REM R1 0.103, Rweak 0.008, Alpha 0.134, Orientation as input
REM Formula found by SHELXT: C20 N10 O10 Mo3 S
CELL 0.71073 8.629 12.1305 17.0785 109.173 104.625 90.077
ZERR 2 0.0003 0.0004 0.0006 0.003 0.003 0.003
LATT 1
SFAC C H Mo N O S
UNIT 38 48 6 20 18 2
DFIX 0.88 0.01 N8 H8
DFIX 0.88 0.01 N4 H4
SADI N1 C5 N1 C5A
SADI C4 C5 C4 C5A
SADI N2 C4 N2 C4A
SADI C4 C5 C4A C5
SADI C4 C5A C4A C5A
SADI 0.01 C4A C5A C4 C5
DELU 0.001 0.001 O5 C2 O7 C6 N1 N3 C10 N6 C12 N9 C19 N10 C18 C4 N2 N2 C3
SIMU 0.01 0.01 3.8 $O
SIMU 0.02 0.04 3.8 C4 C4A C5 C5A
ISOR 0.01 0.01 C1 C4 C6 C9 C18
L.S. 20
PLAN 1
SIZE 0.3 0.2 0.04
TEMP -100.15
BOND $H
list 4
ABIN
fmap 2
acta
REM
REM
REM
WGHT 0.039600 0.114800
FVAR 0.36207 0.33854
MO2 3 0.414190 0.741355 0.732778 11.00000 0.02385 0.02310 =
0.01969 0.00754 0.01314 0.00686
MO1 3 0.646280 0.685336 0.841860 11.00000 0.02169 0.02267 =
0.01833 0.00602 0.01105 0.00356
MO3 3 0.422879 0.526143 0.731995 11.00000 0.02212 0.02140 =
0.01865 0.00526 0.01191 0.00413
S1 6 0.377620 0.685238 0.847265 11.00000 0.02317 0.02402 =
0.01996 0.00624 0.01265 0.00485
O3 5 0.652972 0.534077 0.759019 11.00000 0.02437 0.02347 =
0.02076 0.00513 0.01245 0.00558
O2 5 0.397466 0.592923 0.642141 11.00000 0.02330 0.02596 =
0.02245 0.00657 0.01103 0.00528
O1 5 0.646238 0.763499 0.759172 11.00000 0.02612 0.02329 =
0.02187 0.00594 0.01436 0.00363
O4 5 0.699845 0.634406 0.943963 11.00000 0.02630 0.03694 =
0.02397 0.01558 0.01123 0.00709
O5 5 0.901154 0.695690 0.870949 11.00000 0.02474 0.03669 =
0.02763 0.01183 0.01230 0.00340
O8 5 0.409990 0.821678 0.638619 11.00000 0.04158 0.03072 =
0.02819 0.01327 0.02029 0.01156
O7 5 0.380677 0.906153 0.793844 11.00000 0.05119 0.02564 =
0.03070 0.01035 0.02521 0.01531
N7 4 0.441699 0.364319 0.629123 11.00000 0.02950 0.02470 =
0.02231 0.00516 0.01307 0.00451
N9 4 0.167198 0.463506 0.696871 11.00000 0.03025 0.03134 =
0.02852 0.00572 0.01653 0.00280
N2 4 0.700819 1.011806 1.056764 11.00000 0.04019 0.02966 =
0.02450 0.00161 0.01451 0.00469
PART 1
AFIX 43
H2A 2 0.703037 1.049821 1.110731 21.00000 -1.20000
AFIX 43
PART 0
PART 2
H2B 2 0.681208 1.052559 1.105807 -21.00000 -1.20000
AFIX 0
PART 0
N1 4 0.692090 0.864812 0.939691 11.00000 0.03349 0.02459 =
0.02452 0.00410 0.01458 0.00100
N6 4 0.434296 0.368183 0.928742 11.00000 0.04082 0.04049 =
0.02455 0.01498 0.01443 0.00161
AFIX 43
H6 2 0.401604 0.361395 0.971899 11.00000 -1.20000
AFIX 0
N5 4 0.445164 0.418857 0.817964 11.00000 0.02768 0.02691 =
0.02472 0.00799 0.01322 0.00511
N8 4 0.506090 0.256219 0.512474 11.00000 0.04258 0.03234 =
0.02646 0.00407 0.02059 0.00845
N3 4 0.144711 0.727168 0.682329 11.00000 0.02692 0.04801 =
0.03108 0.01742 0.01745 0.01191
O6 5 1.115590 0.646642 0.951708 11.00000 0.02804 0.09220 =
0.05441 0.03860 0.01198 0.00801
N10 4 -0.085283 0.450455 0.698073 11.00000 0.02994 0.04648 =
0.04818 0.00268 0.01831 -0.00013
AFIX 43
H10 2 -0.174291 0.466663 0.714079 11.00000 -1.20000
AFIX 0
C14 1 0.494731 0.364414 0.561898 11.00000 0.02969 0.02926 =
0.02672 0.00552 0.01351 0.00292
AFIX 43
H14 2 0.520849 0.433128 0.551016 11.00000 -1.20000
AFIX 0
C12 1 0.563297 0.320322 0.902318 11.00000 0.03881 0.04036 =
0.04684 0.02603 0.01256 0.01223
AFIX 43
H12 2 0.635279 0.274182 0.927134 11.00000 -1.20000
AFIX 0
N4 4 -0.110736 0.732838 0.678138 11.00000 0.02705 0.08440 =
0.03818 0.02668 0.01590 0.01724
C8 1 0.037556 0.761695 0.726768 11.00000 0.02901 0.04362 =
0.03287 0.01207 0.01586 0.00837
AFIX 43
H8A 2 0.064942 0.802695 0.787009 11.00000 -1.20000
AFIX 0
O9 5 0.376921 0.986555 0.611660 11.00000 0.14638 0.04640 =
0.06020 0.03429 0.05663 0.03240
C17 1 0.057269 0.505799 0.738921 11.00000 0.02872 0.03170 =
0.03399 0.00751 0.01472 0.00200
AFIX 43
H17 2 0.079990 0.568684 0.792229 11.00000 -1.20000
AFIX 0
C2 1 0.970981 0.656099 0.930893 11.00000 0.02531 0.04823 =
0.02905 0.01415 0.00780 0.00442
C3 1 0.652856 0.899905 1.012192 11.00000 0.04585 0.02903 =
0.02551 0.00475 0.01777 0.00239
AFIX 43
H3 2 0.596176 0.850756 1.031015 11.00000 -1.20000
AFIX 0
PART 1
C4 1 0.746272 1.055587 1.000596 21.00000 0.04065 0.03623 =
0.04167 0.01179 0.01675 -0.00246
AFIX 43
H4A 2 0.769515 1.136039 1.009482 21.00000 -1.20000
AFIX 0
PART 0
C11 1 0.367174 0.426795 0.877524 11.00000 0.03229 0.03490 =
0.02993 0.01539 0.01320 0.00398
AFIX 43
H11 2 0.275432 0.468959 0.882615 11.00000 -1.20000
AFIX 0
C13 1 0.568405 0.351063 0.834834 11.00000 0.04368 0.04183 =
0.04443 0.02406 0.02580 0.01640
AFIX 43
H13 2 0.645915 0.329312 0.802996 11.00000 -1.20000
AFIX 0
C1 1 0.860948 0.613905 0.974091 11.00000 0.02962 0.07050 =
0.04684 0.03607 0.00934 0.00880
AFIX 23
H1A 2 0.867604 0.528896 0.963041 11.00000 -1.20000
H1B 2 0.898026 0.654817 1.037048 11.00000 -1.20000
AFIX 0
C16 1 0.421775 0.248480 0.620571 11.00000 0.07181 0.03439 =
0.04169 0.01234 0.03131 0.00375
AFIX 43
H16 2 0.385394 0.219423 0.658768 11.00000 -1.20000
AFIX 0
C15 1 0.462712 0.181113 0.548079 11.00000 0.07723 0.02698 =
0.04287 0.00752 0.02908 0.00963
AFIX 43
H15 2 0.460862 0.098109 0.527149 11.00000 -1.20000
AFIX 0
C9 1 -0.102556 0.666079 0.597597 11.00000 0.03867 0.12064 =
0.04071 0.02017 0.00716 0.01614
AFIX 43
H9 2 -0.190462 0.628466 0.549139 11.00000 -1.20000
AFIX 0
C19 1 0.083669 0.369659 0.626096 11.00000 0.04001 0.06576 =
0.04688 -0.01903 0.01947 -0.00417
AFIX 43
H19 2 0.128660 0.318105 0.584118 11.00000 -1.20000
AFIX 0
C7 1 0.382671 0.930023 0.659050 11.00000 0.07860 0.03224 =
0.04363 0.02099 0.03746 0.02014
C10 1 0.056599 0.664226 0.600652 11.00000 0.03640 0.12404 =
0.02862 0.01297 0.01279 0.01935
AFIX 43
H10A 2 0.099433 0.625530 0.553714 11.00000 -1.20000
AFIX 0
C18 1 -0.071862 0.363999 0.626959 11.00000 0.03835 0.07243 =
0.05807 -0.01874 0.01681 -0.01060
AFIX 43
H18 2 -0.156255 0.309397 0.585323 11.00000 -1.20000
AFIX 0
C6 1 0.361056 0.983970 0.748880 11.00000 0.10003 0.03573 =
0.04596 0.02177 0.04369 0.02407
AFIX 23
H6A 2 0.440140 1.053226 0.781284 11.00000 -1.20000
H6B 2 0.252099 1.011163 0.744615 11.00000 -1.20000
AFIX 0
H8 2 0.539873 0.233325 0.465543 11.00000 0.03568
H4 2 -0.207866 0.729909 0.684711 11.00000 0.07767
PART 1
C5 1 0.752119 0.965860 0.931608 10.70000 0.05072 0.03988 =
0.02571 0.00056 0.02282 -0.00978
AFIX 43
H5 2 0.790443 0.969939 0.885055 10.70000 -1.20000
AFIX 0
PART 0
PART 2
C5A 1 0.805550 0.954203 0.954544 10.30000 0.04063 0.03789 =
0.03331 0.00386 0.02221 -0.00507
AFIX 43
H5A 2 0.888420 0.946621 0.926079 10.30000 -1.20000
AFIX 0
C4A 1 0.785438 1.052337 1.013403 -21.00000 0.06905 0.04095 =
0.05291 -0.01469 0.04236 -0.02526
AFIX 43
H4AA 2 0.821199 1.130857 1.022737 -21.00000 -1.20000
AFIX 0
HKLF 4
REM exp_17643_a.res in P-1
REM R1 = 0.0388 for 6895 Fo > 4sig(Fo) and 0.0508 for all 8418 data
REM 406 parameters refined using 181 restraints
END
WGHT 0.0396 0.1261
REM Highest difference peak 0.999, deepest hole -0.843, 1-sigma level 0.115
Q1 1 -0.0868 0.7718 0.6116 11.00000 0.05 1.00
REM The information below was added by Olex2.
REM
REM R1 = 0.0388 for 6895 Fo > 4sig(Fo) and 0.0508 for all 25698 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.00, deepest hole -0.84
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0508
REM R1_gt = 0.0388
REM wR_ref = 0.0913
REM GOOF = 1.019
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 25698
REM Reflections_gt = 6895
REM Parameters = n/a
REM Hole = -0.84
REM Peak = 1.00
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.138
_oxdiff_exptl_absorpt_empirical_full_min 0.893
#######################################################################
#
# 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_exp_16981
_database_code_depnum_ccdc_archive 'CCDC 1814437'
_audit_update_record
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_audit_creation_date 2018-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C18.04 H36.04 Mo3 N6 Na2 O18 S, 4(H2 O)'
_chemical_formula_sum 'C18.04 H44.04 Mo3 N6 Na2 O22 S'
_chemical_formula_weight 1062.97
_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 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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 triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.4659(7)
_cell_length_b 12.7032(7)
_cell_length_c 14.8254(9)
_cell_angle_alpha 105.896(5)
_cell_angle_beta 94.713(5)
_cell_angle_gamma 119.364(6)
_cell_volume 1901.1(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 4322
_cell_measurement_temperature 173
_cell_measurement_theta_max 62.0368
_cell_measurement_theta_min 3.2056
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 9.513
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.41865
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour violet
_exptl_crystal_colour_primary violet
_exptl_crystal_density_diffrn 1.857
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1069
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0538
_diffrn_reflns_av_unetI/netI 0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 10608
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full 62.127
_diffrn_reflns_theta_max 62.127
_diffrn_reflns_theta_min 3.208
_diffrn_ambient_temperature 173.0
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -24.00 98.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 32.3066 -19.0000 -90.0000 122
#__ type_ start__ end____ width___ exp.time_
2 omega 47.00 95.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -92.0000 -30.0000 48
#__ type_ start__ end____ width___ exp.time_
3 omega 43.00 69.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -112.0000 -120.0000 26
#__ type_ start__ end____ width___ exp.time_
4 omega 52.00 104.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -92.0000 -180.0000 52
#__ type_ start__ end____ width___ exp.time_
5 omega 23.00 67.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -123.0000 -19.0000 44
#__ type_ start__ end____ width___ exp.time_
6 omega 26.00 63.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -112.0000 30.0000 37
#__ type_ start__ end____ width___ exp.time_
7 omega 73.00 99.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -92.0000 120.0000 26
#__ type_ start__ end____ width___ exp.time_
8 omega 51.00 116.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -38.0000 90.0000 65
#__ type_ start__ end____ width___ exp.time_
9 omega 74.00 128.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -25.0000 30.0000 54
#__ type_ start__ end____ width___ exp.time_
10 omega 91.00 167.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 77.0000 90.0000 76
#__ type_ start__ end____ width___ exp.time_
11 omega 79.00 117.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 112.0000 -120.0000 38
#__ type_ start__ end____ width___ exp.time_
12 omega 71.00 97.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 32.3066 151.0000 -137.0000 26
#__ type_ start__ end____ width___ exp.time_
13 omega 47.00 78.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 32.3066 178.0000 -90.0000 31
#__ type_ start__ end____ width___ exp.time_
14 omega 37.00 171.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 12.0000 60.0000 134
#__ type_ start__ end____ width___ exp.time_
15 omega 40.00 75.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 32.3066 -99.0000 120.0000 35
#__ type_ start__ end____ width___ exp.time_
16 omega 23.00 105.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -50.0000 30.0000 82
#__ type_ start__ end____ width___ exp.time_
17 omega 32.00 58.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -25.0000 30.0000 26
#__ type_ start__ end____ width___ exp.time_
18 omega 21.00 127.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -93.0000 53.4868 106
#__ type_ start__ end____ width___ exp.time_
19 omega 22.00 132.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -92.0000 -90.0000 110
#__ type_ start__ end____ width___ exp.time_
20 omega 21.00 60.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -112.0000 -90.0000 39
#__ type_ start__ end____ width___ exp.time_
21 omega -35.00 37.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 32.3066 -57.0000 -120.0000 72
#__ type_ start__ end____ width___ exp.time_
22 omega -22.00 14.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 32.3066 -99.0000 120.0000 36
#__ type_ start__ end____ width___ exp.time_
23 omega -101.00 -74.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -32.3066 -178.0000 -120.0000 27
#__ type_ start__ end____ width___ exp.time_
24 omega -110.00 -70.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -32.3066 -178.0000 -30.0000 40
#__ type_ start__ end____ width___ exp.time_
25 omega -112.00 -75.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -32.3066 -178.0000 90.0000 37
#__ type_ start__ end____ width___ exp.time_
26 omega -113.00 -85.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -32.3066 178.0000 -150.0000 28
;
_diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5410
_reflns_number_total 5910
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_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 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 1.794
_refine_diff_density_min -1.398
_refine_diff_density_rms 0.206
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.123
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 520
_refine_ls_number_reflns 5910
_refine_ls_number_restraints 119
_refine_ls_R_factor_all 0.0730
_refine_ls_R_factor_gt 0.0686
_refine_ls_restrained_S_all 1.138
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+17.9074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1790
_refine_ls_wR_factor_ref 0.1832
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, {H7A,H7B} of C7, {H1A,H1B} of C1, All C(H,H,H,H,H,H,H,H,H,
H,H,H,H,H,H,H,H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
At 2 times of:
{H8WA,H8WB} of C15A
2. Restrained distances
O2W-H2WB = O2W-H2WA
0.85 with sigma of 0.01
H2WA-H2WB
1.39 with sigma of 0.01
O1W-H1WA = O1W-H1WB
0.85 with sigma of 0.01
H1WA-H1WB
1.39 with sigma of 0.01
O3W-H3WA = O3W-H3WB
0.9 with sigma of 0.01
O7W-H7WA
0.85 with sigma of 0.01
O5W-H5WA = O5W-H5WB
0.9 with sigma of 0.01
H5WA-H5WB
1.39 with sigma of 0.01
O4W-H4WA = O4W-H4WB
0.85 with sigma of 0.01
H4WA-H4WB
1.39 with sigma of 0.01
O8W-H8WA
0.85 with sigma of 0.01
O10W-H10B = O10W-H10A
0.85 with sigma of 0.01
H10B-H10A
1.39 with sigma of 0.01
O9W-H9WA = O9W-H9WB
0.85 with sigma of 0.01
H9WA-H9WB
1.39 with sigma of 0.01
C15A-C13A \\sim C15-C13
with sigma of 0.01
3. Rigid bond restraints
C1
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C15A \\sim C15 \\sim C13A \\sim C13: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C3A) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C13A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
Sof(H1B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
Sof(H1A)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
Sof(C13A)=Sof(H13A)=FVAR(3)
Fixed Sof: C13(0.46) H13(0.46) C15(0.6) H15A(0.6) H15B(0.6) H15C(0.6)
C15A(0.4) H15D(0.4) H15E(0.4) H15F(0.4)
6.a Riding coordinates:
C15A(H9WA,H9WB,H10A,H10B,H8WA,H4WA,H4WB,H7WA,H5WA,H5WB,H7WB,H8WB,H6WA,H6WB,
H3WA,H3WB,H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
C7(H7A), C7(H7B), C1(H1A), C1(H1B), C13(H13), C13A(H13A)
6.c Aromatic/amide H refined with riding coordinates:
N2(H2), N6(H6), N4(H4), C6(H6A), C4(H4A), C16(H16), C18(H18), C11(H11),
C17(H17), C12(H12), C10(H10), C5(H5)
6.d Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C),
C9A(H9AA,H9AB,H9AC), C15A(H15D,H15E,H15F)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_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
Mo1 Mo 0.82418(6) 0.57013(6) 0.22015(5) 0.0170(2) Uani 1 1 d . . . . .
Mo2 Mo 0.79113(7) 0.34903(6) 0.21662(5) 0.0179(2) Uani 1 1 d . . . . .
Mo3 Mo 0.60297(6) 0.38598(6) 0.22225(5) 0.0177(2) Uani 1 1 d . . . . .
S1 S 0.69174(19) 0.37261(19) 0.08710(15) 0.0175(4) Uani 1 1 d . . . . .
Na1 Na 1.1198(3) 1.1753(3) 0.4042(3) 0.0268(8) Uani 1 1 d . . . . .
Na2 Na 0.8875(5) 0.2299(5) 0.4416(4) 0.0511(12) Uani 1 1 d . . . . .
O10 O 0.4445(6) 0.2114(6) 0.1515(5) 0.0265(14) Uani 1 1 d . . . . .
O11 O 0.4864(6) 0.3754(6) 0.3210(5) 0.0251(14) Uani 1 1 d . . . . .
O2 O 0.6789(6) 0.3274(6) 0.3008(4) 0.0221(13) Uani 1 1 d . . . . .
O1 O 0.9163(6) 0.5273(6) 0.3002(5) 0.0236(14) Uani 1 1 d . . . . .
O5 O 0.9543(6) 0.7659(6) 0.3157(5) 0.0242(14) Uani 1 1 d . . . . .
O3 O 0.7134(6) 0.5667(6) 0.3044(5) 0.0216(13) Uani 1 1 d . . . . .
O4 O 0.7894(7) 0.6664(6) 0.1483(5) 0.0269(14) Uani 1 1 d . . . . .
O7 O 0.9079(6) 0.3259(6) 0.1401(5) 0.0276(15) Uani 1 1 d . . . . .
O8 O 0.8825(7) 0.2943(6) 0.3055(5) 0.0285(15) Uani 1 1 d . . . . .
N1 N 0.9830(7) 0.6169(7) 0.1465(6) 0.0247(17) Uani 1 1 d . . . . .
N5 N 0.4918(8) 0.4487(8) 0.1482(6) 0.0267(18) Uani 1 1 d . . . . .
O3W O 0.9400(8) 0.0871(7) 0.4829(5) 0.053(2) Uani 1 1 d D . . . .
O9 O 0.9981(9) 0.2085(9) 0.3052(6) 0.053(2) Uani 1 1 d . . . . .
N2 N 1.0895(8) 0.6691(8) 0.0392(6) 0.0319(19) Uani 1 1 d . . . . .
H2 H 1.1063 0.6794 -0.0153 0.038 Uiso 1 1 calc R . . . .
O12 O 0.3051(8) 0.2512(8) 0.3486(6) 0.055(2) Uani 1 1 d . . . . .
N3 N 0.6673(8) 0.1342(7) 0.1399(6) 0.0248(17) Uani 1 1 d . . . . .
O6 O 1.0541(8) 0.9657(7) 0.3184(6) 0.046(2) Uani 1 1 d . . . . .
O1W O 1.2356(8) 1.1985(7) 0.5550(6) 0.053(2) Uani 1 1 d D . . . .
N6 N 0.3606(8) 0.4428(8) 0.0363(6) 0.0305(19) Uani 1 1 d . . . . .
H6 H 0.3085 0.4173 -0.0198 0.037 Uiso 1 1 calc R . . . .
N4 N 0.5915(8) -0.0584(7) 0.0291(6) 0.0271(18) Uani 1 1 d . . . . .
H4 H 0.5736 -0.1189 -0.0265 0.033 Uiso 1 1 calc R . . . .
O7W O 0.6999(8) 0.0263(10) 0.6116(8) 0.069(3) Uani 1 1 d D . . . .
O9W O 0.4570(8) 0.8180(9) 0.5911(7) 0.056(2) Uani 1 1 d D . . . .
C6 C 1.1088(9) 0.6710(10) 0.1870(8) 0.032(2) Uani 1 1 d . . . . .
H6A H 1.1436 0.6837 0.2513 0.038 Uiso 1 1 calc R . . . .
C4 C 0.9755(9) 0.6169(9) 0.0571(7) 0.029(2) Uani 1 1 d . . . . .
H4A H 0.8983 0.5838 0.0113 0.035 Uiso 1 1 calc R . . . .
C16 C 0.4221(9) 0.3875(10) 0.0589(7) 0.028(2) Uani 1 1 d . . . . .
H16 H 0.4154 0.3130 0.0152 0.034 Uiso 1 1 calc R . . . .
O6W O 0.4381(11) -0.1662(12) 0.3077(9) 0.083(3) Uani 1 1 d . . . . .
C18 C 0.4760(10) 0.5493(10) 0.1853(8) 0.031(2) Uani 1 1 d . . . . .
H18 H 0.5162 0.6117 0.2494 0.038 Uiso 1 1 calc R . . . .
C11 C 0.5561(10) -0.0779(10) 0.1126(7) 0.030(2) Uani 1 1 d . . . . .
H11 H 0.5082 -0.1586 0.1208 0.036 Uiso 1 1 calc R . . . .
C17 C 0.3957(11) 0.5476(10) 0.1184(8) 0.035(2) Uani 1 1 d . . . . .
H17 H 0.3683 0.6067 0.1260 0.042 Uiso 1 1 calc R . . . .
C2 C 0.9641(10) 0.8515(10) 0.2816(8) 0.036(2) Uani 1 1 d . . . . .
C12 C 0.6027(10) 0.0394(9) 0.1789(7) 0.031(2) Uani 1 1 d . . . . .
H12 H 0.5932 0.0559 0.2433 0.037 Uiso 1 1 calc R . . . .
C10 C 0.6574(9) 0.0687(9) 0.0493(7) 0.025(2) Uani 1 1 d . . . . .
H10 H 0.6930 0.1080 0.0045 0.030 Uiso 1 1 calc R . . . .
C8 C 0.9554(11) 0.2613(11) 0.2684(8) 0.037(3) Uani 1 1 d . . . . .
O10W O 0.3576(11) 0.4826(9) 0.4815(7) 0.094(4) Uani 1 1 d D . . . .
C5 C 1.1767(11) 0.7039(10) 0.1222(8) 0.036(2) Uani 1 1 d . . . . .
H5 H 1.2662 0.7430 0.1317 0.043 Uiso 1 1 calc R . . . .
C14 C 0.3778(10) 0.2718(11) 0.2967(8) 0.040(3) Uani 1 1 d . . . . .
O2W O 1.1205(11) 0.4051(13) 0.5061(8) 0.088(4) Uani 1 1 d D . . . .
C7 C 0.9884(12) 0.2925(13) 0.1792(9) 0.048(3) Uani 1 1 d . U . . .
H7A H 1.0727 0.3765 0.2062 0.058 Uiso 0.55(3) 1 calc R . P A 1
H7B H 0.9614 0.2067 0.1298 0.058 Uiso 0.45(3) 1 calc R . P A 2
C1 C 0.8642(14) 0.8037(11) 0.1907(9) 0.055(3) Uani 1 1 d . U . . .
H1A H 0.9153 0.8293 0.1433 0.067 Uiso 0.51(3) 1 calc R . P B 1
H1B H 0.8017 0.8181 0.2213 0.067 Uiso 0.49(3) 1 calc R . P B 2
C13 C 0.3615(19) 0.153(2) 0.2087(17) 0.026(5) Uani 0.46 1 d D U P C 1
H13 H 0.4117 0.1274 0.2431 0.031 Uiso 0.46 1 calc R . P C 1
O8W O 0.4888(14) 0.6964(13) 0.4249(8) 0.119(5) Uani 1 1 d D . . . .
O4W O 1.1266(9) 0.6095(9) 0.4420(6) 0.071(3) Uani 1 1 d D . . . .
O5W O 0.6731(8) 0.0681(8) 0.4324(6) 0.065(3) Uani 1 1 d D . . . .
C3 C 0.806(3) 0.869(2) 0.198(2) 0.060(9) Uani 0.51(3) 1 d . U P B 1
H3A H 0.7960 0.8859 0.1379 0.090 Uiso 0.51(3) 1 calc GR . P B 1
H3B H 0.8569 0.9520 0.2528 0.090 Uiso 0.51(3) 1 calc GR . P B 1
H3C H 0.7216 0.8182 0.2084 0.090 Uiso 0.51(3) 1 calc GR . P B 1
C3A C 0.881(2) 0.877(2) 0.1270(18) 0.045(8) Uani 0.49(3) 1 d . U P B 2
H3AA H 0.9397 0.8704 0.0891 0.067 Uiso 0.49(3) 1 calc GR . P B 2
H3AB H 0.9158 0.9676 0.1661 0.067 Uiso 0.49(3) 1 calc GR . P B 2
H3AC H 0.7983 0.8407 0.0830 0.067 Uiso 0.49(3) 1 calc GR . P B 2
C15 C 0.255(2) 0.0490(19) 0.1758(16) 0.056(5) Uani 0.6 1 d D U P C 1
H15A H 0.2440 0.0037 0.1074 0.084 Uiso 0.6 1 calc GR . P C 1
H15B H 0.1874 0.0677 0.1814 0.084 Uiso 0.6 1 calc GR . P C 1
H15C H 0.2490 -0.0058 0.2129 0.084 Uiso 0.6 1 calc GR . P C 1
C9 C 1.012(3) 0.212(3) 0.1063(19) 0.055(7) Uani 0.55(3) 1 d . U P A 1
H9A H 0.9498 0.1205 0.0944 0.083 Uiso 0.55(3) 1 calc GR . P A 1
H9B H 1.0983 0.2309 0.1287 0.083 Uiso 0.55(3) 1 calc GR . P A 1
H9C H 1.0052 0.2286 0.0461 0.083 Uiso 0.55(3) 1 calc GR . P A 1
C9A C 1.115(3) 0.362(3) 0.194(2) 0.056(9) Uani 0.45(3) 1 d . U P A 2
H9AA H 1.1362 0.3558 0.1308 0.084 Uiso 0.45(3) 1 calc GR . P A 2
H9AB H 1.1535 0.3278 0.2281 0.084 Uiso 0.45(3) 1 calc GR . P A 2
H9AC H 1.1489 0.4527 0.2323 0.084 Uiso 0.45(3) 1 calc GR . P A 2
C15A C 0.2287(7) 0.0891(6) 0.1410(5) 0.041(6) Uani 0.4 1 d D U P C 2
H15D H 0.2037 0.1014 0.0821 0.061 Uiso 0.4 1 calc GR . P C 2
H15E H 0.1652 0.0783 0.1785 0.061 Uiso 0.4 1 calc GR . P C 2
H15F H 0.2336 0.0116 0.1230 0.061 Uiso 0.4 1 calc GR . P C 2
H9WA H 0.4408 0.7721 0.6236 0.049 Uiso 1 1 d DR . . . .
H9WB H 0.3986 0.8296 0.5752 0.049 Uiso 1 1 d DR . . . .
H10A H 0.3117 0.4034 0.4455 0.049 Uiso 1 1 d DR . . . .
H10B H 0.4050 0.4933 0.5311 0.049 Uiso 1 1 d DR . . . .
H8WA H 0.5217 0.7519 0.4820 0.081 Uiso 1 1 d DR . . . .
H4WA H 1.0714 0.5834 0.3891 0.049 Uiso 1 1 d DR . . . .
H4WB H 1.1412 0.5507 0.4407 0.049 Uiso 1 1 d DR . . . .
H7WA H 0.7713 0.0368 0.6341 0.049 Uiso 1 1 d DR . . . .
H5WA H 0.6907 0.0523 0.4818 0.049 Uiso 1 1 d DR . . . .
H5WB H 0.6112 -0.0037 0.3891 0.049 Uiso 1 1 d DR . . . .
H7WB H 0.6217 -0.0395 0.5944 0.049 Uiso 1 1 d R . . . .
H8WB H 0.4913 0.6172 0.4248 0.081 Uiso 1 1 d R . . . .
H6WA H 0.3626 -0.1661 0.2825 0.049 Uiso 1 1 d R . . . .
H6WB H 0.4208 -0.2203 0.3441 0.049 Uiso 1 1 d R . . . .
H3WA H 0.9628 0.1235 0.5539 0.049 Uiso 1 1 d DR . . . .
H3WB H 0.8965 -0.0072 0.4726 0.049 Uiso 1 1 d DR . . . .
H1WA H 1.2826 1.1675 0.5511 0.049 Uiso 1 1 d DR . . . .
H1WB H 1.2790 1.2776 0.5926 0.049 Uiso 1 1 d DR . . . .
H2WA H 1.195(5) 0.419(11) 0.505(7) 0.049 Uiso 1 1 d DR . . . .
H2WB H 1.124(9) 0.453(10) 0.561(4) 0.049 Uiso 1 1 d DR . . . .
C13A C 0.3354(16) 0.1862(17) 0.1915(14) 0.028(6) Uani 0.58(4) 1 d D U P C 2
H13A H 0.3217 0.2466 0.1683 0.034 Uiso 0.58(4) 1 calc R . P C 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
Mo1 0.0191(4) 0.0153(4) 0.0162(4) 0.0079(3) 0.0066(3) 0.0075(3)
Mo2 0.0219(4) 0.0185(4) 0.0170(4) 0.0087(3) 0.0070(3) 0.0121(3)
Mo3 0.0173(4) 0.0174(4) 0.0169(4) 0.0063(3) 0.0069(3) 0.0079(3)
S1 0.0197(10) 0.0161(10) 0.0156(10) 0.0065(8) 0.0053(8) 0.0085(8)
Na1 0.0264(19) 0.0292(19) 0.027(2) 0.0141(16) 0.0107(16) 0.0141(16)
Na2 0.055(3) 0.068(3) 0.051(3) 0.033(3) 0.023(2) 0.040(3)
O10 0.019(3) 0.025(3) 0.028(4) 0.008(3) 0.014(3) 0.006(3)
O11 0.026(3) 0.025(3) 0.024(3) 0.007(3) 0.012(3) 0.013(3)
O2 0.030(3) 0.023(3) 0.023(3) 0.011(3) 0.011(3) 0.019(3)
O1 0.020(3) 0.028(3) 0.025(3) 0.016(3) 0.007(3) 0.011(3)
O5 0.026(3) 0.013(3) 0.024(3) 0.007(3) 0.006(3) 0.003(3)
O3 0.023(3) 0.019(3) 0.026(3) 0.012(3) 0.008(3) 0.011(3)
O4 0.039(4) 0.019(3) 0.019(3) 0.008(3) 0.005(3) 0.013(3)
O7 0.032(4) 0.034(4) 0.024(3) 0.011(3) 0.010(3) 0.022(3)
O8 0.038(4) 0.031(4) 0.026(4) 0.013(3) 0.011(3) 0.024(3)
N1 0.025(4) 0.021(4) 0.023(4) 0.010(3) 0.011(3) 0.006(3)
N5 0.028(4) 0.027(4) 0.029(4) 0.010(4) 0.006(4) 0.018(4)
O3W 0.050(5) 0.071(6) 0.046(5) 0.026(5) 0.016(4) 0.035(5)
O9 0.075(6) 0.075(6) 0.037(5) 0.019(4) 0.008(4) 0.062(6)
N2 0.036(5) 0.024(4) 0.028(5) 0.009(4) 0.017(4) 0.010(4)
O12 0.035(4) 0.049(5) 0.046(5) 0.001(4) 0.028(4) 0.004(4)
N3 0.032(4) 0.023(4) 0.020(4) 0.008(3) 0.008(3) 0.015(4)
O6 0.049(5) 0.025(4) 0.043(5) 0.014(3) 0.009(4) 0.006(4)
O1W 0.073(6) 0.064(6) 0.035(4) 0.002(4) 0.007(4) 0.055(5)
N6 0.031(5) 0.039(5) 0.028(5) 0.017(4) 0.005(4) 0.021(4)
N4 0.030(4) 0.025(4) 0.027(4) 0.005(3) 0.012(4) 0.017(4)
O7W 0.044(5) 0.071(7) 0.078(7) 0.040(6) 0.002(5) 0.017(5)
O9W 0.053(5) 0.064(6) 0.064(6) 0.044(5) 0.021(5) 0.029(5)
C6 0.025(5) 0.031(5) 0.027(5) 0.011(4) 0.009(4) 0.007(4)
C4 0.028(5) 0.025(5) 0.026(5) 0.010(4) 0.012(4) 0.007(4)
C16 0.032(5) 0.034(5) 0.021(5) 0.013(4) 0.008(4) 0.018(5)
O6W 0.064(7) 0.087(8) 0.078(8) 0.029(6) 0.011(6) 0.027(6)
C18 0.035(6) 0.029(5) 0.027(5) 0.007(4) 0.007(4) 0.017(5)
C11 0.033(5) 0.031(5) 0.028(5) 0.012(4) 0.010(4) 0.018(5)
C17 0.046(6) 0.035(6) 0.035(6) 0.012(5) 0.004(5) 0.031(5)
C2 0.038(6) 0.021(5) 0.032(6) 0.008(4) 0.013(5) 0.004(5)
C12 0.044(6) 0.029(5) 0.027(5) 0.014(4) 0.018(5) 0.021(5)
C10 0.025(5) 0.025(5) 0.026(5) 0.007(4) 0.007(4) 0.015(4)
C8 0.047(7) 0.039(6) 0.031(6) 0.003(5) 0.002(5) 0.034(6)
O10W 0.078(8) 0.100(9) 0.068(8) -0.005(7) -0.010(6) 0.045(7)
C5 0.036(6) 0.037(6) 0.038(6) 0.019(5) 0.015(5) 0.018(5)
C14 0.023(5) 0.041(6) 0.037(6) 0.007(5) 0.010(5) 0.007(5)
O2W 0.071(7) 0.104(9) 0.038(6) 0.014(6) 0.013(5) 0.018(7)
C7 0.043(6) 0.068(7) 0.045(6) 0.014(5) 0.003(4) 0.042(5)
C1 0.081(8) 0.029(5) 0.040(6) 0.018(5) -0.003(5) 0.017(5)
C13 0.025(8) 0.029(8) 0.024(8) 0.012(6) 0.009(6) 0.013(6)
O8W 0.116(12) 0.109(11) 0.107(11) 0.024(9) 0.049(10) 0.048(10)
O4W 0.063(6) 0.105(8) 0.050(6) 0.020(6) 0.005(5) 0.054(6)
O5W 0.050(6) 0.062(6) 0.071(7) 0.032(5) 0.008(5) 0.019(5)
C3 0.065(15) 0.044(12) 0.066(15) 0.002(10) -0.023(11) 0.042(11)
C3A 0.050(11) 0.040(10) 0.042(10) 0.027(8) -0.004(7) 0.018(7)
C15 0.057(9) 0.044(8) 0.046(8) 0.014(6) 0.031(7) 0.010(6)
C9 0.070(14) 0.073(14) 0.067(14) 0.043(11) 0.037(10) 0.056(11)
C9A 0.047(14) 0.077(16) 0.056(15) 0.047(12) 0.037(11) 0.027(11)
C15A 0.025(10) 0.050(12) 0.036(12) 0.007(10) 0.014(9) 0.016(9)
C13A 0.021(7) 0.027(8) 0.031(8) 0.013(6) 0.020(6) 0.006(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Mo2 2.6158(9) . ?
Mo1 Mo3 2.6086(10) . ?
Mo1 S1 2.367(2) . ?
Mo1 O1 1.941(6) . ?
Mo1 O5 2.135(6) . ?
Mo1 O3 1.929(6) . ?
Mo1 O4 1.994(6) . ?
Mo1 N1 2.241(8) . ?
Mo2 Mo3 2.6114(9) . ?
Mo2 S1 2.366(2) . ?
Mo2 O2 1.921(6) . ?
Mo2 O1 1.944(6) . ?
Mo2 O7 1.999(7) . ?
Mo2 O8 2.133(6) . ?
Mo2 N3 2.237(8) . ?
Mo3 S1 2.373(2) . ?
Mo3 O10 2.003(6) . ?
Mo3 O11 2.131(6) . ?
Mo3 O2 1.946(6) . ?
Mo3 O3 1.934(6) . ?
Mo3 N5 2.252(8) . ?
Na1 Na2 3.346(6) 1_565 ?
Na1 O3W 2.514(9) 1_565 ?
Na1 O9 2.287(8) 1_565 ?
Na1 O12 2.348(8) 1_665 ?
Na1 O6 2.284(8) . ?
Na1 O1W 2.420(9) . ?
Na1 O2W 2.890(15) 1_565 ?
Na2 Na1 3.346(6) 1_545 ?
Na2 O8 2.383(8) . ?
Na2 O3W 2.409(9) . ?
Na2 O9 2.566(10) . ?
Na2 C8 2.837(13) . ?
Na2 O2W 2.519(13) . ?
Na2 O4W 2.376(10) 2_766 ?
Na2 O5W 2.406(10) . ?
Na2 H5WA 2.6486 . ?
O10 C13 1.44(2) . ?
O10 C13A 1.454(18) . ?
O11 C14 1.268(13) . ?
O5 C2 1.278(12) . ?
O4 C1 1.419(13) . ?
O7 C7 1.406(12) . ?
O8 C8 1.277(13) . ?
N1 C6 1.363(13) . ?
N1 C4 1.321(13) . ?
N5 C16 1.302(13) . ?
N5 C18 1.362(13) . ?
O3W Na1 2.514(9) 1_545 ?
O3W H3WA 0.9785 . ?
O3W H3WB 1.0012 . ?
O9 Na1 2.287(8) 1_545 ?
O9 C8 1.239(13) . ?
N2 H2 0.8800 . ?
N2 C4 1.328(13) . ?
N2 C5 1.378(14) . ?
O12 Na1 2.348(8) 1_445 ?
O12 C14 1.214(14) . ?
N3 C12 1.392(13) . ?
N3 C10 1.331(12) . ?
O6 C2 1.237(13) . ?
O1W H1WA 0.8495 . ?
O1W H1WB 0.8502 . ?
N6 H6 0.8800 . ?
N6 C16 1.344(13) . ?
N6 C17 1.379(14) . ?
N4 H4 0.8800 . ?
N4 C11 1.393(13) . ?
N4 C10 1.328(12) . ?
O7W H7WA 0.8550 . ?
O7W H7WB 0.8707 . ?
O9W H9WA 0.8171 . ?
O9W H9WB 0.8396 . ?
C6 H6A 0.9500 . ?
C6 C5 1.350(15) . ?
C4 H4A 0.9500 . ?
C16 H16 0.9500 . ?
O6W H6WA 0.9843 . ?
O6W H6WB 0.9424 . ?
C18 H18 0.9500 . ?
C18 C17 1.339(14) . ?
C11 H11 0.9500 . ?
C11 C12 1.333(14) . ?
C17 H17 0.9500 . ?
C2 C1 1.507(17) . ?
C12 H12 0.9500 . ?
C10 H10 0.9500 . ?
C8 C7 1.515(18) . ?
O10W H10A 0.8463 . ?
O10W H10B 0.8395 . ?
C5 H5 0.9500 . ?
C14 C13 1.61(3) . ?
C14 C13A 1.51(2) . ?
O2W Na1 2.890(15) 1_545 ?
O2W H2WA 0.856(10) . ?
O2W H2WB 0.850(10) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C7 C9 1.43(3) . ?
C7 C9A 1.34(3) . ?
C1 H1A 1.0000 . ?
C1 H1B 1.0000 . ?
C1 C3 1.34(3) . ?
C1 C3A 1.45(2) . ?
C13 H13 1.0000 . ?
C13 C15 1.255(17) . ?
O8W H8WA 0.8450 . ?
O8W H8WB 1.0216 . ?
O4W Na2 2.376(10) 2_766 ?
O4W H4WA 0.8627 . ?
O4W H4WB 0.8461 . ?
O5W H5WA 0.8495 . ?
O5W H5WB 0.8644 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?
C15A C13A 1.254(15) . ?
C13A H13A 1.0000 . ?
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
Mo3 Mo1 Mo2 59.98(3) . . ?
S1 Mo1 Mo2 56.44(5) . . ?
S1 Mo1 Mo3 56.71(6) . . ?
O1 Mo1 Mo2 47.72(19) . . ?
O1 Mo1 Mo3 92.76(18) . . ?
O1 Mo1 S1 103.0(2) . . ?
O1 Mo1 O5 85.4(3) . . ?
O1 Mo1 O4 160.4(3) . . ?
O1 Mo1 N1 84.7(3) . . ?
O5 Mo1 Mo2 133.02(17) . . ?
O5 Mo1 Mo3 133.31(18) . . ?
O5 Mo1 S1 167.31(18) . . ?
O5 Mo1 N1 81.8(3) . . ?
O3 Mo1 Mo2 93.26(17) . . ?
O3 Mo1 Mo3 47.61(18) . . ?
O3 Mo1 S1 103.00(19) . . ?
O3 Mo1 O1 93.1(3) . . ?
O3 Mo1 O5 85.8(3) . . ?
O3 Mo1 O4 97.1(3) . . ?
O3 Mo1 N1 167.6(3) . . ?
O4 Mo1 Mo2 147.33(18) . . ?
O4 Mo1 Mo3 106.5(2) . . ?
O4 Mo1 S1 90.99(19) . . ?
O4 Mo1 O5 78.8(2) . . ?
O4 Mo1 N1 81.7(3) . . ?
N1 Mo1 Mo2 94.3(2) . . ?
N1 Mo1 Mo3 144.6(2) . . ?
N1 Mo1 S1 89.4(2) . . ?
Mo3 Mo2 Mo1 59.87(3) . . ?
S1 Mo2 Mo1 56.47(5) . . ?
S1 Mo2 Mo3 56.68(5) . . ?
O2 Mo2 Mo1 93.32(17) . . ?
O2 Mo2 Mo3 47.93(17) . . ?
O2 Mo2 S1 103.30(19) . . ?
O2 Mo2 O1 93.0(3) . . ?
O2 Mo2 O7 161.5(3) . . ?
O2 Mo2 O8 86.0(3) . . ?
O2 Mo2 N3 86.2(3) . . ?
O1 Mo2 Mo1 47.63(18) . . ?
O1 Mo2 Mo3 92.61(18) . . ?
O1 Mo2 S1 102.90(18) . . ?
O1 Mo2 O7 95.8(3) . . ?
O1 Mo2 O8 86.7(3) . . ?
O1 Mo2 N3 168.5(3) . . ?
O7 Mo2 Mo1 104.64(19) . . ?
O7 Mo2 Mo3 147.33(19) . . ?
O7 Mo2 S1 90.65(19) . . ?
O7 Mo2 O8 78.3(3) . . ?
O7 Mo2 N3 82.0(3) . . ?
O8 Mo2 Mo1 134.28(18) . . ?
O8 Mo2 Mo3 133.84(19) . . ?
O8 Mo2 S1 166.10(18) . . ?
O8 Mo2 N3 81.8(3) . . ?
N3 Mo2 Mo1 143.8(2) . . ?
N3 Mo2 Mo3 95.3(2) . . ?
N3 Mo2 S1 88.4(2) . . ?
Mo1 Mo3 Mo2 60.15(3) . . ?
S1 Mo3 Mo1 56.50(5) . . ?
S1 Mo3 Mo2 56.44(5) . . ?
O10 Mo3 Mo1 148.45(18) . . ?
O10 Mo3 Mo2 105.59(18) . . ?
O10 Mo3 S1 91.97(19) . . ?
O10 Mo3 O11 78.0(2) . . ?
O10 Mo3 N5 81.7(3) . . ?
O11 Mo3 Mo1 133.03(17) . . ?
O11 Mo3 Mo2 132.44(18) . . ?
O11 Mo3 S1 168.01(18) . . ?
O11 Mo3 N5 84.6(3) . . ?
O2 Mo3 Mo1 92.94(19) . . ?
O2 Mo3 Mo2 47.11(18) . . ?
O2 Mo3 S1 102.27(19) . . ?
O2 Mo3 O10 95.4(3) . . ?
O2 Mo3 O11 85.5(3) . . ?
O2 Mo3 N5 170.0(3) . . ?
O3 Mo3 Mo1 47.45(19) . . ?
O3 Mo3 Mo2 93.28(18) . . ?
O3 Mo3 S1 102.65(19) . . ?
O3 Mo3 O10 160.5(3) . . ?
O3 Mo3 O11 85.8(2) . . ?
O3 Mo3 O2 94.0(3) . . ?
O3 Mo3 N5 86.2(3) . . ?
N5 Mo3 Mo1 94.4(2) . . ?
N5 Mo3 Mo2 142.9(2) . . ?
N5 Mo3 S1 87.4(2) . . ?
Mo1 S1 Mo3 66.78(6) . . ?
Mo2 S1 Mo1 67.10(6) . . ?
Mo2 S1 Mo3 66.87(6) . . ?
O3W Na1 Na2 45.9(2) 1_565 1_565 ?
O3W Na1 O2W 78.2(3) 1_565 1_565 ?
O9 Na1 Na2 50.0(2) 1_565 1_565 ?
O9 Na1 O3W 88.6(3) 1_565 1_565 ?
O9 Na1 O12 100.6(4) 1_565 1_665 ?
O9 Na1 O1W 157.4(3) 1_565 . ?
O9 Na1 O2W 69.1(3) 1_565 1_565 ?
O12 Na1 Na2 142.0(3) 1_665 1_565 ?
O12 Na1 O3W 170.7(4) 1_665 1_565 ?
O12 Na1 O1W 90.9(3) 1_665 . ?
O12 Na1 O2W 104.9(4) 1_665 1_565 ?
O6 Na1 Na2 115.6(3) . 1_565 ?
O6 Na1 O3W 87.4(3) . 1_565 ?
O6 Na1 O9 101.1(3) . 1_565 ?
O6 Na1 O12 90.9(3) . 1_665 ?
O6 Na1 O1W 98.1(3) . . ?
O6 Na1 O2W 162.5(4) . 1_565 ?
O1W Na1 Na2 110.3(2) . 1_565 ?
O1W Na1 O3W 80.3(3) . 1_565 ?
O1W Na1 O2W 89.2(3) . 1_565 ?
O2W Na1 Na2 46.9(3) 1_565 1_565 ?
Na1 Na2 H5WA 116.7 1_545 . ?
O8 Na2 Na1 94.3(2) . 1_545 ?
O8 Na2 O3W 135.7(3) . . ?
O8 Na2 O9 52.4(2) . . ?
O8 Na2 C8 26.5(3) . . ?
O8 Na2 O2W 88.9(4) . . ?
O8 Na2 O5W 108.1(3) . . ?
O8 Na2 H5WA 126.6 . . ?
O3W Na2 Na1 48.5(2) . 1_545 ?
O3W Na2 O9 84.9(3) . . ?
O3W Na2 C8 110.2(3) . . ?
O3W Na2 O2W 87.9(4) . . ?
O3W Na2 H5WA 70.2 . . ?
O9 Na2 Na1 43.05(19) . 1_545 ?
O9 Na2 C8 25.9(3) . . ?
O9 Na2 H5WA 131.0 . . ?
C8 Na2 Na1 68.1(2) . 1_545 ?
C8 Na2 H5WA 134.9 . . ?
O2W Na2 Na1 57.0(4) . 1_545 ?
O2W Na2 O9 71.7(4) . . ?
O2W Na2 C8 78.7(4) . . ?
O2W Na2 H5WA 144.2 . . ?
O4W Na2 Na1 135.0(3) 2_766 1_545 ?
O4W Na2 O8 99.6(3) 2_766 . ?
O4W Na2 O3W 123.3(3) 2_766 . ?
O4W Na2 O9 139.8(4) 2_766 . ?
O4W Na2 C8 121.2(4) 2_766 . ?
O4W Na2 O2W 80.6(4) 2_766 . ?
O4W Na2 O5W 90.4(4) 2_766 . ?
O4W Na2 H5WA 88.1 2_766 . ?
O5W Na2 Na1 125.3(3) . 1_545 ?
O5W Na2 O3W 84.1(3) . . ?
O5W Na2 O9 123.4(4) . . ?
O5W Na2 C8 119.3(4) . . ?
O5W Na2 O2W 161.9(4) . . ?
O5W Na2 H5WA 18.6 . . ?
C13 O10 Mo3 116.8(9) . . ?
C13A O10 Mo3 115.0(7) . . ?
C14 O11 Mo3 116.9(6) . . ?
Mo2 O2 Mo3 85.0(2) . . ?
Mo1 O1 Mo2 84.6(2) . . ?
C2 O5 Mo1 114.9(6) . . ?
Mo1 O3 Mo3 84.9(3) . . ?
C1 O4 Mo1 116.7(6) . . ?
C7 O7 Mo2 117.9(7) . . ?
Mo2 O8 Na2 147.0(4) . . ?
C8 O8 Mo2 114.9(7) . . ?
C8 O8 Na2 97.0(6) . . ?
C6 N1 Mo1 128.1(7) . . ?
C4 N1 Mo1 125.4(7) . . ?
C4 N1 C6 105.6(8) . . ?
C16 N5 Mo3 124.9(6) . . ?
C16 N5 C18 105.8(8) . . ?
C18 N5 Mo3 129.2(7) . . ?
Na1 O3W H3WA 116.0 1_545 . ?
Na1 O3W H3WB 116.6 1_545 . ?
Na2 O3W Na1 85.6(3) . 1_545 ?
Na2 O3W H3WA 101.5 . . ?
Na2 O3W H3WB 137.9 . . ?
H3WA O3W H3WB 99.6 . . ?
Na1 O9 Na2 87.0(3) 1_545 . ?
C8 O9 Na1 162.4(8) . 1_545 ?
C8 O9 Na2 89.4(7) . . ?
C4 N2 H2 126.4 . . ?
C4 N2 C5 107.2(9) . . ?
C5 N2 H2 126.4 . . ?
C14 O12 Na1 163.0(8) . 1_445 ?
C12 N3 Mo2 128.5(6) . . ?
C10 N3 Mo2 126.0(7) . . ?
C10 N3 C12 104.7(8) . . ?
C2 O6 Na1 147.1(8) . . ?
Na1 O1W H1WA 117.2 . . ?
Na1 O1W H1WB 110.1 . . ?
H1WA O1W H1WB 109.6 . . ?
C16 N6 H6 126.9 . . ?
C16 N6 C17 106.2(8) . . ?
C17 N6 H6 126.9 . . ?
C11 N4 H4 126.5 . . ?
C10 N4 H4 126.5 . . ?
C10 N4 C11 107.0(8) . . ?
H7WA O7W H7WB 132.7 . . ?
H9WA O9W H9WB 114.0 . . ?
N1 C6 H6A 125.1 . . ?
C5 C6 N1 109.9(9) . . ?
C5 C6 H6A 125.1 . . ?
N1 C4 N2 111.5(9) . . ?
N1 C4 H4A 124.3 . . ?
N2 C4 H4A 124.3 . . ?
N5 C16 N6 111.7(9) . . ?
N5 C16 H16 124.1 . . ?
N6 C16 H16 124.1 . . ?
H6WA O6W H6WB 112.3 . . ?
N5 C18 H18 124.9 . . ?
C17 C18 N5 110.2(9) . . ?
C17 C18 H18 124.9 . . ?
N4 C11 H11 126.8 . . ?
C12 C11 N4 106.3(9) . . ?
C12 C11 H11 126.8 . . ?
N6 C17 H17 127.0 . . ?
C18 C17 N6 106.0(8) . . ?
C18 C17 H17 127.0 . . ?
O5 C2 C1 116.1(9) . . ?
O6 C2 O5 121.8(10) . . ?
O6 C2 C1 121.9(10) . . ?
N3 C12 H12 125.0 . . ?
C11 C12 N3 110.1(9) . . ?
C11 C12 H12 125.0 . . ?
N3 C10 H10 124.1 . . ?
N4 C10 N3 111.9(9) . . ?
N4 C10 H10 124.1 . . ?
O8 C8 Na2 56.5(5) . . ?
O8 C8 C7 116.6(9) . . ?
O9 C8 Na2 64.8(7) . . ?
O9 C8 O8 121.2(11) . . ?
O9 C8 C7 122.2(10) . . ?
C7 C8 Na2 172.4(7) . . ?
H10A O10W H10B 110.9 . . ?
N2 C5 H5 127.1 . . ?
C6 C5 N2 105.8(9) . . ?
C6 C5 H5 127.1 . . ?
O11 C14 C13 113.9(11) . . ?
O11 C14 C13A 114.4(10) . . ?
O12 C14 O11 123.3(10) . . ?
O12 C14 C13 120.1(11) . . ?
O12 C14 C13A 121.4(11) . . ?
Na1 O2W H2WA 66(8) 1_545 . ?
Na1 O2W H2WB 145(9) 1_545 . ?
Na2 O2W Na1 76.1(4) . 1_545 ?
Na2 O2W H2WA 142(7) . . ?
Na2 O2W H2WB 103(7) . . ?
H2WA O2W H2WB 109.2(18) . . ?
O7 C7 C8 110.8(9) . . ?
O7 C7 H7A 103.3 . . ?
O7 C7 H7B 103.6 . . ?
O7 C7 C9 113.1(13) . . ?
C8 C7 H7A 103.3 . . ?
C8 C7 H7B 103.6 . . ?
C9 C7 C8 120.7(14) . . ?
C9 C7 H7A 103.3 . . ?
C9A C7 O7 122.9(17) . . ?
C9A C7 C8 109.9(15) . . ?
C9A C7 H7B 103.6 . . ?
O4 C1 C2 112.2(9) . . ?
O4 C1 H1A 103.3 . . ?
O4 C1 H1B 98.8 . . ?
O4 C1 C3A 118.0(13) . . ?
C2 C1 H1A 103.3 . . ?
C2 C1 H1B 98.8 . . ?
C3 C1 O4 118.9(17) . . ?
C3 C1 C2 113.5(15) . . ?
C3 C1 H1A 103.3 . . ?
C3A C1 C2 122.9(14) . . ?
C3A C1 H1B 98.8 . . ?
O10 C13 C14 105.8(13) . . ?
O10 C13 H13 100.8 . . ?
C14 C13 H13 100.8 . . ?
C15 C13 O10 125(2) . . ?
C15 C13 C14 118(2) . . ?
C15 C13 H13 100.8 . . ?
H8WA O8W H8WB 108.6 . . ?
Na2 O4W H4WA 106.1 2_766 . ?
Na2 O4W H4WB 138.2 2_766 . ?
H4WA O4W H4WB 108.9 . . ?
Na2 O5W H5WA 97.1 . . ?
Na2 O5W H5WB 136.4 . . ?
H5WA O5W H5WB 108.3 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C3A H3AA 109.5 . . ?
C1 C3A H3AB 109.5 . . ?
C1 C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9A H9AA 109.5 . . ?
C7 C9A H9AB 109.5 . . ?
C7 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C13A C15A H15D 109.5 . . ?
C13A C15A H15E 109.5 . . ?
C13A C15A H15F 109.5 . . ?
O10 C13A C14 110.7(11) . . ?
O10 C13A H13A 93.3 . . ?
C14 C13A H13A 93.3 . . ?
C15A C13A O10 117.6(14) . . ?
C15A C13A C14 130.6(14) . . ?
C15A C13A H13A 93.3 . . ?
_shelx_res_file
;
exp_16981.res created by SHELXL-2014/7
TITL exp_16981_a.res in P-1
REM Old TITL exp_16981 in P-1
REM SHELXT solution in P-1
REM R1 0.102, Rweak 0.011, Alpha 0.087, Orientation as input
REM Formula found by SHELXT: C17 O14 S N16 Mo3
CELL 1.54184 12.4659 12.7032 14.8254 105.896 94.713 119.364
ZERR 2 0.0007 0.0007 0.0009 0.005 0.005 0.006
LATT 1
SFAC C H Mo N Na O S
UNIT 36.08 88.08 6 12 4 44 2
DFIX 0.85 0.01 O2W H2Wb O2W H2Wa
DFIX 1.39 0.01 H2Wa H2Wb
DFIX 0.85 0.01 O1W H1Wa O1W H1Wb
DFIX 1.39 0.01 H1Wa H1Wb
DFIX 0.9 0.01 O3W H3Wa O3W H3Wb
DFIX 0.85 0.01 O7W H7Wa
DFIX 0.9 0.01 O5W H5Wa O5W H5Wb
DFIX 1.39 0.01 H5Wa H5Wb
DFIX 0.85 0.01 O4W H4Wa O4W H4Wb
DFIX 1.39 0.01 H4Wa H4Wb
DFIX 0.85 0.01 O8W H8Wa
DFIX 0.85 0.01 O10W H10b O10W H10a
DFIX 1.39 0.01 H10b H10a
DFIX 0.85 0.01 O9W H9Wa O9W H9Wb
DFIX 1.39 0.01 H9Wa H9Wb
SADI 0.01 C15A C13A C15 C13
DELU 0.01 0.005 C1
SIMU 0.02 0.04 3.8 C15A C15 C13A C13
ISOR 0.01 0.02 C3A C3 C9A C9 C15A
ISOR 0.01 0.01 C3A C15
ISOR 0.01 0.01 C1 C7 C13 C13A
L.S. 20
PLAN 1
TEMP -100.15
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.082100 17.907400
FVAR 0.34516 0.50956 0.54820 0.57788
MO1 3 0.824175 0.570130 0.220146 11.00000 0.01909 0.01530 =
0.01621 0.00789 0.00655 0.00749
MO2 3 0.791125 0.349027 0.216616 11.00000 0.02192 0.01853 =
0.01702 0.00870 0.00698 0.01210
MO3 3 0.602972 0.385981 0.222251 11.00000 0.01732 0.01738 =
0.01690 0.00626 0.00686 0.00788
S1 7 0.691745 0.372611 0.087104 11.00000 0.01973 0.01614 =
0.01557 0.00651 0.00527 0.00845
NA1 5 1.119810 1.175333 0.404227 11.00000 0.02645 0.02924 =
0.02712 0.01409 0.01067 0.01414
NA2 5 0.887491 0.229890 0.441577 11.00000 0.05509 0.06758 =
0.05066 0.03271 0.02284 0.03965
O10 6 0.444497 0.211367 0.151467 11.00000 0.01938 0.02494 =
0.02791 0.00789 0.01447 0.00648
O11 6 0.486413 0.375432 0.321035 11.00000 0.02555 0.02496 =
0.02352 0.00661 0.01175 0.01284
O2 6 0.678863 0.327434 0.300786 11.00000 0.03020 0.02338 =
0.02268 0.01095 0.01135 0.01926
O1 6 0.916297 0.527297 0.300237 11.00000 0.02028 0.02767 =
0.02466 0.01562 0.00694 0.01073
O5 6 0.954319 0.765877 0.315670 11.00000 0.02579 0.01294 =
0.02394 0.00686 0.00619 0.00333
O3 6 0.713412 0.566653 0.304388 11.00000 0.02297 0.01946 =
0.02581 0.01238 0.00793 0.01145
O4 6 0.789408 0.666399 0.148321 11.00000 0.03944 0.01877 =
0.01899 0.00769 0.00526 0.01303
O7 6 0.907853 0.325879 0.140142 11.00000 0.03248 0.03376 =
0.02387 0.01134 0.00974 0.02193
O8 6 0.882538 0.294338 0.305505 11.00000 0.03765 0.03140 =
0.02640 0.01314 0.01068 0.02366
N1 4 0.982963 0.616914 0.146481 11.00000 0.02457 0.02077 =
0.02261 0.00976 0.01062 0.00611
N5 4 0.491795 0.448652 0.148156 11.00000 0.02829 0.02712 =
0.02856 0.00975 0.00567 0.01782
O3W 6 0.940021 0.087110 0.482889 11.00000 0.04983 0.07068 =
0.04589 0.02588 0.01563 0.03519
O9 6 0.998134 0.208503 0.305249 11.00000 0.07513 0.07497 =
0.03747 0.01900 0.00805 0.06159
N2 4 1.089536 0.669068 0.039250 11.00000 0.03610 0.02434 =
0.02753 0.00907 0.01687 0.00970
AFIX 43
H2 2 1.106289 0.679445 -0.015309 11.00000 -1.20000
AFIX 0
O12 6 0.305148 0.251199 0.348584 11.00000 0.03526 0.04914 =
0.04591 0.00103 0.02819 0.00370
N3 4 0.667339 0.134211 0.139910 11.00000 0.03180 0.02291 =
0.02041 0.00842 0.00772 0.01476
O6 6 1.054111 0.965723 0.318351 11.00000 0.04911 0.02526 =
0.04307 0.01429 0.00883 0.00567
O1W 6 1.235577 1.198515 0.554995 11.00000 0.07345 0.06408 =
0.03469 0.00232 0.00699 0.05486
N6 4 0.360645 0.442825 0.036259 11.00000 0.03094 0.03897 =
0.02775 0.01656 0.00529 0.02114
AFIX 43
H6 2 0.308524 0.417253 -0.019782 11.00000 -1.20000
AFIX 0
N4 4 0.591502 -0.058410 0.029135 11.00000 0.03037 0.02465 =
0.02713 0.00534 0.01198 0.01668
AFIX 43
H4 2 0.573643 -0.118851 -0.026485 11.00000 -1.20000
AFIX 0
O7W 6 0.699939 0.026254 0.611577 11.00000 0.04431 0.07068 =
0.07796 0.03991 0.00219 0.01660
O9W 6 0.457006 0.817954 0.591096 11.00000 0.05340 0.06440 =
0.06370 0.04391 0.02101 0.02853
C6 1 1.108840 0.671005 0.186989 11.00000 0.02541 0.03103 =
0.02734 0.01129 0.00928 0.00656
AFIX 43
H6A 2 1.143632 0.683674 0.251297 11.00000 -1.20000
AFIX 0
C4 1 0.975531 0.616929 0.057058 11.00000 0.02751 0.02480 =
0.02572 0.01008 0.01208 0.00682
AFIX 43
H4A 2 0.898348 0.583809 0.011290 11.00000 -1.20000
AFIX 0
C16 1 0.422061 0.387538 0.058914 11.00000 0.03235 0.03357 =
0.02120 0.01299 0.00779 0.01755
AFIX 43
H16 2 0.415404 0.312970 0.015154 11.00000 -1.20000
AFIX 0
O6W 6 0.438114 -0.166185 0.307703 11.00000 0.06364 0.08664 =
0.07783 0.02939 0.01055 0.02699
C18 1 0.476020 0.549290 0.185297 11.00000 0.03537 0.02914 =
0.02674 0.00720 0.00675 0.01708
AFIX 43
H18 2 0.516246 0.611668 0.249424 11.00000 -1.20000
AFIX 0
C11 1 0.556073 -0.077880 0.112637 11.00000 0.03335 0.03148 =
0.02779 0.01212 0.01039 0.01759
AFIX 43
H11 2 0.508233 -0.158639 0.120789 11.00000 -1.20000
AFIX 0
C17 1 0.395665 0.547630 0.118413 11.00000 0.04565 0.03545 =
0.03509 0.01208 0.00427 0.03073
AFIX 43
H17 2 0.368316 0.606682 0.126009 11.00000 -1.20000
AFIX 0
C2 1 0.964095 0.851492 0.281587 11.00000 0.03811 0.02099 =
0.03166 0.00838 0.01296 0.00404
C12 1 0.602683 0.039428 0.178868 11.00000 0.04363 0.02859 =
0.02747 0.01446 0.01845 0.02107
AFIX 43
H12 2 0.593164 0.055929 0.243251 11.00000 -1.20000
AFIX 0
C10 1 0.657353 0.068651 0.049325 11.00000 0.02502 0.02451 =
0.02611 0.00683 0.00742 0.01541
AFIX 43
H10 2 0.693041 0.108005 0.004477 11.00000 -1.20000
AFIX 0
C8 1 0.955362 0.261289 0.268448 11.00000 0.04740 0.03937 =
0.03065 0.00253 0.00222 0.03382
O10W 6 0.357627 0.482641 0.481456 11.00000 0.07789 0.09985 =
0.06802 -0.00520 -0.01011 0.04538
C5 1 1.176741 0.703907 0.122158 11.00000 0.03554 0.03682 =
0.03831 0.01925 0.01460 0.01816
AFIX 43
H5 2 1.266191 0.743013 0.131710 11.00000 -1.20000
AFIX 0
C14 1 0.377814 0.271826 0.296651 11.00000 0.02256 0.04104 =
0.03749 0.00697 0.01045 0.00708
O2W 6 1.120540 0.405059 0.506075 11.00000 0.07115 0.10401 =
0.03847 0.01419 0.01342 0.01776
C7 1 0.988356 0.292507 0.179170 11.00000 0.04303 0.06822 =
0.04475 0.01416 0.00289 0.04222
PART 1
AFIX 13
H7A 2 1.072668 0.376456 0.206246 31.00000 -1.20000
AFIX 13
PART 0
PART 2
H7B 2 0.961407 0.206731 0.129767 -31.00000 -1.20000
AFIX 0
PART 0
C1 1 0.864217 0.803694 0.190687 11.00000 0.08077 0.02872 =
0.03966 0.01811 -0.00286 0.01707
PART 1
AFIX 13
H1A 2 0.915260 0.829279 0.143290 21.00000 -1.20000
AFIX 13
PART 0
PART 2
H1B 2 0.801667 0.818071 0.221317 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C13 1 0.361540 0.153208 0.208707 10.46000 0.02543 0.02917 =
0.02365 0.01245 0.00858 0.01303
AFIX 13
H13 2 0.411696 0.127367 0.243147 10.46000 -1.20000
AFIX 0
PART 0
O8W 6 0.488778 0.696407 0.424928 11.00000 0.11642 0.10871 =
0.10718 0.02373 0.04915 0.04781
O4W 6 1.126596 0.609483 0.442002 11.00000 0.06266 0.10506 =
0.05021 0.01994 0.00535 0.05383
O5W 6 0.673095 0.068054 0.432435 11.00000 0.05029 0.06157 =
0.07135 0.03161 0.00817 0.01866
PART 1
C3 1 0.805724 0.869378 0.197921 21.00000 0.06517 0.04438 =
0.06620 0.00177 -0.02284 0.04189
AFIX 137
H3A 2 0.795974 0.885916 0.137900 21.00000 -1.50000
H3B 2 0.856910 0.951996 0.252775 21.00000 -1.50000
H3C 2 0.721560 0.818203 0.208374 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C3A 1 0.880845 0.876519 0.127014 -21.00000 0.04962 0.04039 =
0.04217 0.02743 -0.00375 0.01846
AFIX 137
H3AA 2 0.939664 0.870351 0.089059 -21.00000 -1.50000
H3AB 2 0.915801 0.967572 0.166073 -21.00000 -1.50000
H3AC 2 0.798280 0.840740 0.082977 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C15 1 0.254634 0.048974 0.175767 10.60000 0.05651 0.04422 =
0.04551 0.01377 0.03148 0.00996
AFIX 137
H15A 2 0.244009 0.003741 0.107356 10.60000 -1.50000
H15B 2 0.187439 0.067654 0.181367 10.60000 -1.50000
H15C 2 0.248999 -0.005839 0.212863 10.60000 -1.50000
AFIX 0
C9 1 1.012337 0.211726 0.106347 31.00000 0.07000 0.07263 =
0.06685 0.04298 0.03708 0.05649
AFIX 137
H9A 2 0.949833 0.120511 0.094372 31.00000 -1.50000
H9B 2 1.098349 0.230892 0.128748 31.00000 -1.50000
H9C 2 1.005223 0.228550 0.046138 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C9A 1 1.115306 0.361903 0.193583 -31.00000 0.04732 0.07670 =
0.05623 0.04710 0.03672 0.02706
AFIX 137
H9AA 2 1.136201 0.355835 0.130799 -31.00000 -1.50000
H9AB 2 1.153513 0.327816 0.228132 -31.00000 -1.50000
H9AC 2 1.148927 0.452745 0.232343 -31.00000 -1.50000
AFIX 0
C15A 1 0.228650 0.089052 0.141002 10.40000 0.02489 0.04988 =
0.03648 0.00724 0.01422 0.01598
AFIX 137
H15D 2 0.203747 0.101385 0.082144 10.40000 -1.50000
H15E 2 0.165222 0.078261 0.178483 10.40000 -1.50000
H15F 2 0.233576 0.011631 0.122957 10.40000 -1.50000
AFIX 3
PART 0
H9WA 2 0.440830 0.772092 0.623641 11.00000 -1.20000
H9WB 2 0.398560 0.829592 0.575171 11.00000 -1.20000
H10A 2 0.311650 0.403362 0.445542 11.00000 -1.20000
H10B 2 0.405000 0.493302 0.531121 11.00000 -1.20000
H8WA 2 0.521690 0.751942 0.482002 11.00000 -2.00000
H4WA 2 1.071350 0.583402 0.389102 11.00000 -1.20000
H4WB 2 1.141180 0.550732 0.440652 11.00000 -1.20000
H7WA 2 0.771300 0.036772 0.634132 11.00000 -1.20000
H5WA 2 0.690690 0.052302 0.481842 11.00000 -1.20000
H5WB 2 0.611150 -0.003668 0.389082 11.00000 -1.20000
H7WB 2 0.621660 -0.039518 0.594372 11.00000 -1.20000
H8WB 2 0.491330 0.617192 0.424772 11.00000 -2.00000
H6WA 2 0.362610 -0.166118 0.282472 11.00000 -1.20000
H6WB 2 0.420790 -0.220328 0.344122 11.00000 -1.20000
H3WA 2 0.962820 0.123492 0.553872 11.00000 -1.20000
H3WB 2 0.896500 -0.007238 0.472582 11.00000 -1.20000
H1WA 2 1.282610 1.167522 0.551122 11.00000 -1.20000
H1WB 2 1.278980 1.277572 0.592592 11.00000 -1.20000
AFIX 0
H2WA 2 1.195026 0.419312 0.505396 11.00000 -1.20000
H2WB 2 1.123855 0.452529 0.560644 11.00000 -1.20000
PART 2
C13A 1 0.335393 0.186162 0.191452 41.00000 0.02124 0.02685 =
0.03078 0.01254 0.01962 0.00641
AFIX 13
H13A 2 0.321683 0.246612 0.168311 41.00000 -1.20000
AFIX 0
HKLF 4
REM exp_16981_a.res in P-1
REM R1 = 0.0686 for 5410 Fo > 4sig(Fo) and 0.0730 for all 5910 data
REM 520 parameters refined using 119 restraints
END
WGHT 0.0821 17.9190
REM Highest difference peak 1.794, deepest hole -1.398, 1-sigma level 0.206
Q1 1 0.3405 0.6604 0.3873 11.00000 0.05 1.79
;
_shelx_res_checksum 98786
_olex2_exptl_crystal_mounting_method set
_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_exp_15827
_database_code_depnum_ccdc_archive 'CCDC 1814439'
_audit_update_record
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_audit_creation_date 2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '0.5(C32 H24 Mo12 Na12 O64)'
_chemical_formula_sum 'C16 H12 Mo6 Na6 O32'
_chemical_formula_weight 1429.84
_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 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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 orthorhombic
_space_group_IT_number 44
_space_group_name_H-M_alt 'I m m 2'
_space_group_name_Hall 'I 2 -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z'
'-x, y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
_cell_length_a 15.0786(10)
_cell_length_b 18.8242(10)
_cell_length_c 7.2176(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2048.7(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2274
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 62.0955
_cell_measurement_theta_min 3.7528
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 16.168
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.22525
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.318
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 1364
_exptl_crystal_size_max 0.04
_exptl_crystal_size_mid 0.02
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0465
_diffrn_reflns_av_unetI/netI 0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 5
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 5531
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full 62.185
_diffrn_reflns_theta_max 62.185
_diffrn_reflns_theta_min 3.756
_diffrn_ambient_temperature 173
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -105.00 -74.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- -32.3066 -178.0000 90.0000 31
#__ type_ start__ end____ width___ exp.time_
2 omega -104.00 -58.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- -32.3066 -178.0000 -90.0000 46
#__ type_ start__ end____ width___ exp.time_
3 omega -75.00 -39.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- -32.3066 97.0000 115.0000 36
#__ type_ start__ end____ width___ exp.time_
4 omega -113.00 -69.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- -32.3066 178.0000 -180.0000 44
#__ type_ start__ end____ width___ exp.time_
5 omega -42.00 72.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- 32.3066 -19.0000 150.0000 114
#__ type_ start__ end____ width___ exp.time_
6 omega -38.00 26.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- 32.3066 -57.0000 -60.0000 64
#__ type_ start__ end____ width___ exp.time_
7 omega -39.00 64.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- 32.3066 -38.0000 60.0000 103
#__ type_ start__ end____ width___ exp.time_
8 omega 23.00 49.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -50.0000 -150.0000 26
#__ type_ start__ end____ width___ exp.time_
9 omega 23.00 91.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -112.0000 150.0000 68
#__ type_ start__ end____ width___ exp.time_
10 omega 74.00 101.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -50.0000 120.0000 27
#__ type_ start__ end____ width___ exp.time_
11 omega 68.00 162.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 64.0000 -90.0000 94
#__ type_ start__ end____ width___ exp.time_
12 omega 115.00 165.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 50.0000 -150.0000 50
#__ type_ start__ end____ width___ exp.time_
13 omega 71.00 99.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -92.0000 -120.0000 28
#__ type_ start__ end____ width___ exp.time_
14 omega 117.00 153.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 64.0000 -120.0000 36
#__ type_ start__ end____ width___ exp.time_
15 omega 99.00 169.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 25.0000 -30.0000 70
#__ type_ start__ end____ width___ exp.time_
16 omega 32.00 67.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -112.0000 -150.0000 35
#__ type_ start__ end____ width___ exp.time_
17 omega 27.00 136.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -92.0000 -30.0000 109
#__ type_ start__ end____ width___ exp.time_
18 omega 53.00 120.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -50.0000 -150.0000 67
#__ type_ start__ end____ width___ exp.time_
19 omega 64.00 168.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 38.0000 30.0000 104
#__ type_ start__ end____ width___ exp.time_
20 omega 83.00 132.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -92.0000 120.0000 49
#__ type_ start__ end____ width___ exp.time_
21 omega 34.00 120.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -50.0000 -30.0000 86
#__ type_ start__ end____ width___ exp.time_
22 omega 24.00 53.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -50.0000 120.0000 29
#__ type_ start__ end____ width___ exp.time_
23 omega 102.00 134.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 112.0000 -30.0000 32
#__ type_ start__ end____ width___ exp.time_
24 omega 74.00 101.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 94.5000 -93.0000 -151.7662 27
;
_diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0399832000
_diffrn_orient_matrix_UB_12 0.0884728000
_diffrn_orient_matrix_UB_13 -0.0378755000
_diffrn_orient_matrix_UB_21 -0.0623435000
_diffrn_orient_matrix_UB_22 -0.0510719000
_diffrn_orient_matrix_UB_23 -0.0667095000
_diffrn_orient_matrix_UB_31 -0.2001062000
_diffrn_orient_matrix_UB_32 -0.0020187000
_diffrn_orient_matrix_UB_33 0.0285808000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage 0.837
_reflns_Friedel_fraction_full 0.993
_reflns_Friedel_fraction_max 0.993
_reflns_number_gt 1405
_reflns_number_total 1451
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 61.08
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_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 2.745
_refine_diff_density_min -1.161
_refine_diff_density_rms 0.215
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.03(6)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 149
_refine_ls_number_reflns 1451
_refine_ls_number_restraints 153
_refine_ls_R_factor_all 0.0559
_refine_ls_R_factor_gt 0.0546
_refine_ls_restrained_S_all 1.029
_refine_ls_shift/su_max 0.071
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1163P)^2^+15.2479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1511
_refine_ls_wR_factor_ref 0.1541
_refine_special_details
;
Refined as a 2-component inversion twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.97(6)
0.03(6)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
3. Rigid bond restraints
O2, C2, Mo2, O1
with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
O5, C4, O4, C4
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C1 \\sim C3 \\sim C4 \\sim C2: within 3.8A with sigma of 0.005 and sigma for
terminal atoms of 0.01
O1 \\sim O10 \\sim O9 \\sim O7 \\sim O2 \\sim O5 \\sim O8 \\sim O3 \\sim O4
\\sim O6: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
C1(H1)
5.b Secondary CH2 refined with riding coordinates:
C3(H3A,H3B)
;
_atom_sites_solution_hydrogens geom
_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
Mo1 Mo 0.41521(8) 0.5000 0.4413(3) 0.0277(5) Uani 1 2 d S T P . .
Mo2 Mo 0.27671(8) 0.43103(6) 0.7776(2) 0.0379(5) Uani 1 1 d . U . . .
O1 O 0.3099(8) 0.4266(5) 0.4804(19) 0.0398(16) Uani 1 1 d . U . . .
O10 O 0.5000 0.5742(7) 0.493(3) 0.036(3) Uani 1 2 d S TU P . .
O9 O 0.4022(10) 0.5000 0.206(3) 0.037(3) Uani 1 2 d S TU P . .
O7 O 0.3762(10) 0.5000 0.751(3) 0.0386(19) Uani 1 2 d S TU P . .
O2 O 0.3669(7) 0.3462(5) 0.7414(19) 0.0421(17) Uani 1 1 d . U . . .
O5 O 0.0996(8) 0.2875(7) 0.529(2) 0.050(2) Uani 1 1 d . U . . .
O8 O 0.1890(11) 0.5000 0.713(3) 0.043(2) Uani 1 2 d S TU P . .
O3 O 0.4059(8) 0.2590(6) 0.549(2) 0.045(2) Uani 1 1 d . U . . .
O4 O 0.1838(8) 0.3575(6) 0.691(2) 0.0457(17) Uani 1 1 d . U . . .
O6 O 0.2688(8) 0.4122(7) 1.003(2) 0.049(3) Uani 1 1 d . U . . .
C1 C 0.3232(8) 0.3534(7) 0.418(3) 0.036(2) Uani 1 1 d . U . . .
H1 H 0.3607 0.3512 0.3041 0.043 Uiso 1 1 calc R . . . .
C3 C 0.2337(9) 0.3190(8) 0.388(3) 0.037(2) Uani 1 1 d . U . . .
H3A H 0.2058 0.3422 0.2794 0.044 Uiso 1 1 calc R . . . .
H3B H 0.2439 0.2687 0.3547 0.044 Uiso 1 1 calc R . . . .
C4 C 0.1685(10) 0.3208(8) 0.543(3) 0.038(2) Uani 1 1 d . U . . .
C2 C 0.3690(10) 0.3151(8) 0.586(3) 0.037(2) Uani 1 1 d . U . . .
Na1 Na 0.5000 0.2187(7) 0.781(2) 0.073(4) Uani 1 2 d S T P . .
Na2 Na 0.0000 0.2718(12) 0.788(2) 0.105(6) Uani 1 2 d S T P . .
Na3 Na 0.5000 0.362(2) 0.063(7) 0.24(3) Uani 1 2 d S T P . .
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
Mo1 0.0247(8) 0.0214(7) 0.0369(10) 0.000 0.0032(8) 0.000
Mo2 0.0419(7) 0.0370(7) 0.0347(8) 0.0026(6) 0.0027(6) -0.0065(5)
O1 0.034(3) 0.034(3) 0.052(4) -0.003(3) -0.001(3) -0.003(2)
O10 0.035(5) 0.022(5) 0.050(6) -0.002(4) 0.000 0.000
O9 0.040(6) 0.017(5) 0.055(8) 0.000 -0.005(6) 0.000
O7 0.037(4) 0.030(3) 0.048(4) 0.000 -0.001(3) 0.000
O2 0.039(3) 0.035(3) 0.053(4) -0.002(3) 0.000(3) -0.003(3)
O5 0.033(4) 0.052(5) 0.064(6) -0.009(5) 0.000(4) -0.007(4)
O8 0.038(4) 0.038(4) 0.051(4) 0.000 0.001(4) 0.000
O3 0.038(4) 0.038(4) 0.059(5) -0.002(4) 0.000(4) 0.004(3)
O4 0.040(3) 0.042(3) 0.055(4) -0.004(3) 0.001(3) -0.006(3)
O6 0.054(5) 0.042(4) 0.052(6) 0.001(5) 0.004(4) -0.009(4)
C1 0.026(4) 0.033(4) 0.048(6) 0.003(4) 0.001(4) -0.006(4)
C3 0.030(4) 0.030(4) 0.049(6) 0.000(4) 0.000(4) -0.008(4)
C4 0.029(4) 0.035(4) 0.051(6) 0.001(4) 0.001(4) -0.006(4)
C2 0.029(4) 0.031(4) 0.051(6) 0.001(4) -0.002(4) -0.006(4)
Na1 0.043(5) 0.084(7) 0.092(10) 0.040(8) 0.000 0.000
Na2 0.046(6) 0.212(19) 0.057(8) 0.025(12) 0.000 0.000
Na3 0.096(16) 0.29(4) 0.33(6) -0.20(4) 0.000 0.000
_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
Mo1 Mo1 2.557(3) 2_665 ?
Mo1 O1 2.123(11) 3_565 ?
Mo1 O1 2.123(11) . ?
Mo1 O10 1.930(10) . ?
Mo1 O10 1.930(10) 2_665 ?
Mo1 O9 1.71(2) . ?
Mo1 O7 2.31(2) . ?
Mo2 Mo2 2.597(2) 3_565 ?
Mo2 O1 2.204(14) . ?
Mo2 O7 1.993(11) . ?
Mo2 O2 2.113(11) . ?
Mo2 O8 1.911(13) . ?
Mo2 O4 2.067(12) . ?
Mo2 O6 1.669(15) . ?
O1 C1 1.465(17) . ?
O10 Mo1 1.930(10) 2_665 ?
O7 Mo2 1.993(11) 3_565 ?
O2 C2 1.27(2) . ?
O5 C4 1.22(2) . ?
O5 Na1 2.335(19) 6_554 ?
O5 Na2 2.418(19) . ?
O8 Mo2 1.911(13) 3_565 ?
O3 C2 1.22(2) . ?
O3 Na1 2.324(17) . ?
O3 Na2 2.430(19) 6_554 ?
O4 C4 1.29(2) . ?
C1 H1 1.0000 . ?
C1 C3 1.512(18) . ?
C1 C2 1.57(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.49(2) . ?
Na1 O5 2.335(19) 6 ?
Na1 O5 2.335(19) 7 ?
Na1 O3 2.324(17) 4_655 ?
Na1 C2 3.032(19) 4_655 ?
Na1 Na2 3.57(2) 6_554 ?
Na1 Na2 3.66(2) 6 ?
Na1 Na3 3.37(3) 1_556 ?
Na2 O5 2.418(19) 4 ?
Na2 O3 2.430(19) 6 ?
Na2 O3 2.430(19) 7_455 ?
Na2 Na1 3.57(2) 6 ?
Na2 Na1 3.66(2) 6_554 ?
Na2 Na3 2.99(6) 6 ?
Na3 Na1 3.37(3) 1_554 ?
Na3 Na2 2.99(6) 6_554 ?
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 Mo1 Mo1 138.4(3) . 2_665 ?
O1 Mo1 Mo1 138.4(3) 3_565 2_665 ?
O1 Mo1 O1 81.1(6) 3_565 . ?
O1 Mo1 O7 71.4(4) 3_565 . ?
O1 Mo1 O7 71.4(4) . . ?
O10 Mo1 Mo1 48.5(3) 2_665 2_665 ?
O10 Mo1 Mo1 48.5(3) . 2_665 ?
O10 Mo1 O1 90.0(4) 2_665 . ?
O10 Mo1 O1 160.2(7) 2_665 3_565 ?
O10 Mo1 O1 160.2(7) . . ?
O10 Mo1 O1 90.0(4) . 3_565 ?
O10 Mo1 O10 92.8(6) 2_665 . ?
O10 Mo1 O7 89.0(6) . . ?
O10 Mo1 O7 89.0(6) 2_665 . ?
O9 Mo1 Mo1 96.6(5) . 2_665 ?
O9 Mo1 O1 92.7(5) . 3_565 ?
O9 Mo1 O1 92.7(5) . . ?
O9 Mo1 O10 105.4(7) . 2_665 ?
O9 Mo1 O10 105.4(7) . . ?
O9 Mo1 O7 158.7(6) . . ?
O7 Mo1 Mo1 104.7(4) . 2_665 ?
O1 Mo2 Mo2 92.1(2) . 3_565 ?
O7 Mo2 Mo2 49.4(3) . 3_565 ?
O7 Mo2 O1 76.2(6) . . ?
O7 Mo2 O2 89.8(4) . . ?
O7 Mo2 O4 156.6(7) . . ?
O2 Mo2 Mo2 139.1(3) . 3_565 ?
O2 Mo2 O1 72.9(5) . . ?
O8 Mo2 Mo2 47.2(4) . 3_565 ?
O8 Mo2 O1 86.8(6) . . ?
O8 Mo2 O7 93.2(5) . . ?
O8 Mo2 O2 158.2(6) . . ?
O8 Mo2 O4 84.9(5) . . ?
O4 Mo2 Mo2 132.1(3) . 3_565 ?
O4 Mo2 O1 80.4(5) . . ?
O4 Mo2 O2 83.8(5) . . ?
O6 Mo2 Mo2 102.3(5) . 3_565 ?
O6 Mo2 O1 163.0(5) . . ?
O6 Mo2 O7 106.5(7) . . ?
O6 Mo2 O2 90.3(6) . . ?
O6 Mo2 O8 109.5(7) . . ?
O6 Mo2 O4 96.0(6) . . ?
Mo1 O1 Mo2 106.0(5) . . ?
C1 O1 Mo1 118.0(9) . . ?
C1 O1 Mo2 111.4(10) . . ?
Mo1 O10 Mo1 83.0(5) . 2_665 ?
Mo2 O7 Mo1 106.5(7) 3_565 . ?
Mo2 O7 Mo1 106.5(7) . . ?
Mo2 O7 Mo2 81.3(6) 3_565 . ?
C2 O2 Mo2 118.4(11) . . ?
C4 O5 Na1 129.8(14) . 6_554 ?
C4 O5 Na2 121.7(13) . . ?
Na1 O5 Na2 100.7(6) 6_554 . ?
Mo2 O8 Mo2 85.6(7) 3_565 . ?
C2 O3 Na1 113.9(13) . . ?
C2 O3 Na2 129.7(13) . 6_554 ?
Na1 O3 Na2 97.2(6) . 6_554 ?
C4 O4 Mo2 136.9(11) . . ?
O1 C1 H1 111.6 . . ?
O1 C1 C3 108.9(11) . . ?
O1 C1 C2 104.9(14) . . ?
C3 C1 H1 111.6 . . ?
C3 C1 C2 108.0(13) . . ?
C2 C1 H1 111.6 . . ?
C1 C3 H3A 107.8 . . ?
C1 C3 H3B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
C4 C3 C1 118.0(16) . . ?
C4 C3 H3A 107.8 . . ?
C4 C3 H3B 107.8 . . ?
O5 C4 O4 120.0(16) . . ?
O5 C4 C3 119.0(17) . . ?
O4 C4 C3 120.9(13) . . ?
O2 C2 C1 117.3(13) . . ?
O3 C2 O2 127.0(17) . . ?
O3 C2 C1 115.6(16) . . ?
O5 Na1 O5 80.0(8) 7 6 ?
O5 Na1 C2 88.1(5) 7 4_655 ?
O5 Na1 C2 143.6(8) 6 4_655 ?
O5 Na1 Na2 140.0(4) 6 6_554 ?
O5 Na1 Na2 40.5(4) 6 6 ?
O5 Na1 Na2 40.5(4) 7 6 ?
O5 Na1 Na2 140.0(4) 7 6_554 ?
O5 Na1 Na3 65.1(9) 7 1_556 ?
O5 Na1 Na3 65.1(9) 6 1_556 ?
O3 Na1 O5 100.1(5) . 6 ?
O3 Na1 O5 100.1(5) 4_655 7 ?
O3 Na1 O5 163.8(8) 4_655 6 ?
O3 Na1 O5 163.8(8) . 7 ?
O3 Na1 O3 75.3(8) 4_655 . ?
O3 Na1 C2 82.3(6) . 4_655 ?
O3 Na1 C2 21.6(5) 4_655 4_655 ?
O3 Na1 Na2 42.5(5) 4_655 6_554 ?
O3 Na1 Na2 134.8(6) 4_655 6 ?
O3 Na1 Na2 42.5(5) . 6_554 ?
O3 Na1 Na2 134.8(6) . 6 ?
O3 Na1 Na3 100.0(9) 4_655 1_556 ?
O3 Na1 Na3 100.0(9) . 1_556 ?
C2 Na1 Na2 60.3(5) 4_655 6_554 ?
C2 Na1 Na2 115.8(6) 4_655 6 ?
C2 Na1 Na3 78.6(8) 4_655 1_556 ?
Na2 Na1 Na2 174.3(8) 6_554 6 ?
Na3 Na1 Na2 50.1(11) 1_556 6 ?
Na3 Na1 Na2 124.1(11) 1_556 6_554 ?
O5 Na2 O5 76.8(8) 4 . ?
O5 Na2 O3 173.0(11) 4 6 ?
O5 Na2 O3 105.5(5) 4 7_455 ?
O5 Na2 O3 105.5(5) . 6 ?
O5 Na2 O3 173.0(11) . 7_455 ?
O5 Na2 Na1 140.1(5) 4 6 ?
O5 Na2 Na1 38.8(4) . 6_554 ?
O5 Na2 Na1 38.8(4) 4 6_554 ?
O5 Na2 Na1 140.1(5) . 6 ?
O5 Na2 Na3 71.5(8) . 6 ?
O5 Na2 Na3 71.5(8) 4 6 ?
O3 Na2 O3 71.5(7) 6 7_455 ?
O3 Na2 Na1 141.9(5) 6 6_554 ?
O3 Na2 Na1 40.3(4) 6 6 ?
O3 Na2 Na1 40.3(4) 7_455 6 ?
O3 Na2 Na1 141.9(5) 7_455 6_554 ?
O3 Na2 Na3 102.8(9) 6 6 ?
O3 Na2 Na3 102.8(9) 7_455 6 ?
Na1 Na2 Na1 174.3(8) 6 6_554 ?
Na3 Na2 Na1 125.8(9) 6 6 ?
Na3 Na2 Na1 59.9(8) 6 6_554 ?
Na2 Na3 Na1 69.9(9) 6_554 1_554 ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 -0.257 149.9 50.8 5H2O
2 0.500 0.000 -0.026 149.9 50.8 5H2O
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4 17 3 -0.2035 2.8453
4 18 0 -8.7813 0.5241
4 18 2 6.0691 5.0597
4 18 4 -0.7106 -1.3335
4 19 1 -1.6801 7.0872
4 19 3 -0.6850 0.6321
4 20 0 -0.2695 0.9540
4 20 2 2.4904 1.5919
5 0 1 -1.2372 -4.7520
5 1 0 -26.8868 -0.8386
5 2 1 -1.9438 -4.8745
5 3 0 1.4610 -0.1012
5 3 2 3.6972 -7.3880
5 4 1 -2.5120 -5.5805
5 5 0 26.6981 0.3464
5 5 2 -3.5770 -11.5457
5 5 4 -3.6387 -3.1596
5 6 1 -0.2441 -6.5031
5 7 0 23.5230 0.1624
5 7 2 -4.1225 -9.8240
5 7 4 -0.7183 0.4596
5 8 1 4.5028 -5.1190
5 8 3 3.5466 -3.2779
5 9 0 0.2911 -0.1700
5 9 2 2.2642 -3.7580
5 9 4 2.7866 2.1884
5 10 1 8.0870 -0.1135
5 10 3 -0.0555 -5.8389
5 11 0 -15.5181 -0.1197
5 11 2 8.8288 1.0306
5 11 4 2.1261 0.0053
5 12 1 7.6912 5.0023
5 12 3 -2.8293 -6.8092
5 12 5 -3.1150 0.0964
5 13 0 -10.9034 0.1757
5 13 2 8.9382 1.3147
5 13 4 -1.5391 -3.3068
5 14 1 4.4440 4.9894
5 14 3 -1.8167 -6.5041
5 14 5 -3.1691 -0.3818
5 15 0 2.4501 0.1964
5 15 2 2.9218 -1.0780
5 15 4 -3.1677 -3.7769
5 16 1 1.6430 -0.3027
5 16 3 1.3538 -5.0544
5 17 0 7.9211 -0.2286
5 17 2 -2.8989 -2.4610
5 17 4 -1.0131 -1.3369
5 18 1 0.7958 -5.1328
5 18 3 2.6208 -2.1162
5 19 0 3.3448 -0.7351
5 19 2 -3.5961 -1.4907
5 20 1 0.7280 -4.7376
6 0 0 38.5782 2.1649
6 1 1 8.9150 -7.6618
6 2 0 26.0204 1.3703
6 2 2 -11.3342 -5.9404
6 3 1 6.3081 -8.1413
6 4 0 1.6848 0.2633
6 4 2 -6.0796 1.8950
6 4 4 3.0123 6.9725
6 5 1 2.0482 -7.4097
6 6 0 -10.1461 -0.2161
6 6 2 -3.4242 6.5750
6 6 4 1.5668 4.7348
6 7 1 -2.1964 -5.4933
6 7 3 -7.5657 6.9170
6 8 0 -1.7537 -0.0595
6 8 2 -5.9689 4.9188
6 8 4 -1.9342 2.1895
6 9 1 -4.4496 -4.8725
6 9 3 -3.1562 7.5881
6 9 5 3.5914 2.1922
6 10 0 12.0754 0.0900
6 10 2 -10.8265 0.1062
6 10 4 -3.2345 1.8201
6 11 1 -3.7548 -6.3431
6 11 3 1.8546 7.6463
6 11 5 4.5359 0.9383
6 12 0 14.2534 -0.0647
6 12 2 -12.3663 -2.7838
6 12 4 -0.7785 3.5250
6 13 1 -1.2941 -6.8023
6 13 3 3.6000 7.2721
6 13 5 4.7235 0.1843
6 14 0 4.4791 -0.2232
6 14 2 -8.0163 -2.0549
6 14 4 2.1843 4.5696
6 15 1 0.4726 -3.3496
6 15 3 1.0714 6.1127
6 16 0 -4.6078 -0.0875
6 16 2 -1.0294 0.1079
6 16 4 2.1689 3.2201
6 17 1 0.2983 2.0175
6 17 3 -2.1455 3.3923
6 18 0 -4.8340 0.2291
6 18 2 2.9781 1.0634
6 19 1 -0.6840 4.3859
6 20 0 -0.0286 0.4307
7 0 1 -5.5370 7.9259
7 1 0 -28.3481 -1.7487
7 1 2 6.9613 6.2612
7 2 1 -4.2468 8.8523
7 3 0 -14.5741 -0.7349
7 3 2 4.7418 2.7552
7 3 4 1.1034 -4.8162
7 4 1 -1.3495 10.1032
7 5 0 -0.8043 0.0948
7 5 2 2.6810 -1.3011
7 5 4 1.0927 -5.2407
7 6 1 1.4131 9.2423
7 6 3 11.0716 -5.1189
7 6 5 -4.8082 -4.1193
7 7 0 1.1752 0.2223
7 7 2 3.3061 -2.7728
7 7 4 2.4618 -4.8275
7 8 1 2.5320 6.6376
7 8 3 7.6362 -5.7183
7 8 5 -3.9537 -2.7096
7 9 0 -5.9949 0.0046
7 9 2 6.5292 -1.2018
7 9 4 3.5437 -3.9209
7 10 1 1.6378 4.6862
7 10 3 1.1072 -5.2466
7 10 5 -3.9298 -1.6279
7 11 0 -10.4087 -0.0490
7 11 2 9.1969 1.0770
7 11 4 2.5606 -3.2562
7 12 1 -0.2175 3.9632
7 12 3 -4.7987 -5.2139
7 12 5 -4.2507 -0.9388
7 13 0 -5.8473 0.0655
7 13 2 7.9580 1.5869
7 13 4 0.1524 -2.9456
7 14 1 -1.2954 2.4916
7 14 3 -5.7026 -5.1114
7 14 5 -3.6223 -0.3447
7 15 0 2.2253 0.0860
7 15 2 2.9580 0.2021
7 15 4 -1.3339 -2.4061
7 16 1 -0.7291 -0.6729
7 16 3 -2.0477 -3.4978
7 17 0 5.2784 -0.0152
7 17 2 -1.8310 -1.1857
7 18 1 0.5743 -3.2499
7 18 3 1.2961 -0.7004
7 19 0 2.1231 -0.0708
8 0 0 15.1057 0.5352
8 1 1 -3.8863 -2.5466
8 1 5 0.4827 5.2423
8 2 0 10.2963 0.2376
8 2 2 1.5825 1.8568
8 3 1 -3.3799 -3.6192
8 3 5 1.7502 4.7453
8 4 0 0.7991 -0.1562
8 4 2 3.4740 0.4579
8 4 4 -4.5410 0.5623
8 5 1 -2.5942 -4.0203
8 5 3 -9.7974 -1.4302
8 5 5 2.4565 3.1778
8 6 0 -4.1337 -0.2469
8 6 2 4.2488 -0.0038
8 6 4 -4.1718 2.2287
8 7 1 -1.7891 -2.7152
8 7 3 -9.2789 0.8868
8 7 5 1.8417 1.1426
8 8 0 -1.1272 -0.0654
8 8 2 2.4531 0.3837
8 8 4 -3.3254 3.2605
8 9 1 -0.8959 -0.8178
8 9 3 -4.8593 0.8928
8 9 5 1.2201 0.2376
8 10 0 4.2489 0.0730
8 10 2 -1.0263 0.4779
8 10 4 -2.2817 2.6330
8 11 1 0.0850 0.0753
8 11 3 2.4532 1.5357
8 11 5 1.6499 0.7426
8 12 0 4.7686 0.0616
8 12 2 -3.3024 0.1972
8 12 4 -1.2266 1.0792
8 13 1 0.6706 0.1501
8 13 3 7.4728 2.8464
8 13 5 2.2646 1.1084
8 14 0 0.0050 0.0709
8 14 2 -2.2589 0.4607
8 14 4 -0.3021 0.1447
8 15 1 0.3737 0.8142
8 15 3 6.5305 2.6992
8 16 0 -4.1820 0.1723
8 16 2 0.9085 1.2788
8 16 4 0.1926 0.1272
8 17 1 -0.4461 2.1558
8 17 3 2.0167 0.7159
8 18 0 -3.5206 0.2023
8 18 2 2.7115 1.4839
9 0 5 0.9300 -2.4717
9 1 0 -3.5436 0.8584
9 2 1 7.6662 -0.2542
9 2 5 0.3088 -2.2748
9 3 0 2.5743 0.4841
9 3 2 -5.4110 -2.6196
9 3 4 4.8124 3.3568
9 4 1 4.3495 -1.1000
9 4 3 6.0066 6.3688
9 4 5 -0.3743 -1.1094
9 5 0 8.4718 0.1300
9 5 2 -8.4426 0.6118
9 5 4 4.8959 2.7483
9 6 1 1.5520 -2.3348
9 6 3 5.9952 3.0270
9 6 5 0.3792 1.0402
9 7 0 8.1363 -0.0468
9 7 2 -9.2699 0.5283
9 7 4 3.0486 1.0171
9 8 1 0.4562 -3.2806
9 8 3 4.7082 2.4536
9 8 5 1.7791 2.2732
9 9 0 2.1975 -0.0612
9 9 2 -6.8363 -1.1873
9 9 4 0.7861 0.0520
9 10 1 0.4418 -3.1314
9 10 3 0.2993 1.4922
9 10 5 1.8413 1.1523
9 11 0 -3.0500 -0.0152
9 11 2 -2.7848 -1.6635
9 11 4 -0.0523 0.7825
9 12 1 0.4904 -1.8981
9 12 3 -5.1879 -0.8106
9 12 5 0.4023 -0.7871
9 13 0 -2.8725 -0.0403
9 13 2 -0.1309 -0.8501
9 13 4 0.3689 1.7339
9 14 1 0.3999 -0.7683
9 14 3 -7.2853 -2.0443
9 15 0 0.9448 -0.2002
9 15 2 -0.3614 -0.4630
9 15 4 0.6435 1.4354
9 16 1 0.4055 -0.8597
9 16 3 -4.6614 -0.8142
9 17 0 3.1665 -0.3755
9 17 2 -1.9115 -0.7819
9 18 1 0.3662 -1.6378
10 0 0 1.0520 -1.5544
10 0 2 -0.4355 3.2304
10 1 1 -6.3995 -1.2570
10 1 5 0.4207 -0.2637
10 2 0 -2.0332 -0.8305
10 2 2 1.3514 1.6808
10 2 4 -2.1094 -3.2439
10 3 1 -3.8091 0.1688
10 3 5 0.6228 -0.5925
10 4 0 -8.1260 0.0447
10 4 2 5.3694 -0.8193
10 4 4 -3.4125 -4.7903
10 5 1 -0.9268 2.1650
10 5 3 -2.0829 -3.2621
10 5 5 -0.3129 -1.8778
10 6 0 -10.7868 0.3506
10 6 2 8.6417 -0.6572
10 6 4 -2.6269 -4.9278
10 7 1 0.2031 3.5403
10 7 3 -0.6841 -2.7625
10 7 5 -2.4373 -3.2193
10 8 0 -6.7543 0.1476
10 8 2 8.9148 1.7441
10 8 4 -0.1090 -3.8901
10 9 1 -0.3338 3.5404
10 9 3 0.4590 -2.3471
10 9 5 -3.7512 -2.6948
10 10 0 0.5191 -0.0937
10 10 2 6.2166 2.8174
10 10 4 1.5267 -3.1937
10 11 1 -1.0171 2.1867
10 11 3 2.6760 -0.2842
10 11 5 -2.8342 -0.4759
10 12 0 4.4824 -0.1443
10 12 2 2.6275 1.2028
10 12 4 0.9997 -2.9851
10 13 1 -0.9211 0.4209
10 13 3 4.6961 1.6877
10 14 0 2.6196 -0.0566
10 14 2 0.5673 -0.7498
10 14 4 -0.2840 -2.2402
10 15 1 -0.4238 -0.3408
10 15 3 4.3611 1.3307
10 16 0 -1.3368 0.1022
10 16 2 0.7510 -0.8839
10 17 1 -0.1423 0.4100
11 0 1 1.0445 1.9440
11 0 5 -0.9295 1.2433
11 1 0 0.5564 1.1815
11 1 2 1.7831 2.4004
11 2 1 0.5070 1.9216
11 2 5 -1.0635 1.1516
11 3 0 4.1617 0.0724
11 3 2 -0.6490 2.4434
11 3 4 1.2731 3.9183
11 4 1 -0.4429 1.5994
11 4 3 1.3078 1.4503
11 4 5 -0.7606 1.3280
11 5 0 7.5452 -0.5411
11 5 2 -3.5843 1.0674
11 5 4 1.7382 5.3714
11 6 1 -0.8719 0.8892
11 6 3 -2.3020 1.0562
11 6 5 0.8143 1.9879
11 7 0 6.5015 -0.3069
11 7 2 -5.1297 -1.6686
11 7 4 0.5300 5.6224
11 8 1 -0.4374 0.0810
11 8 3 -3.1340 1.2707
11 8 5 2.7428 2.1033
11 9 0 0.9663 0.1289
11 9 2 -4.7849 -3.1227
11 9 4 -1.1071 4.8761
11 10 1 0.2483 -0.2101
11 10 3 -2.4450 0.4240
11 10 5 3.1754 0.9603
11 11 0 -4.2258 0.2520
11 11 2 -3.1238 -1.5127
11 11 4 -1.4430 3.6891
11 12 1 0.3909 0.3034
11 12 3 -2.0148 -1.1296
11 13 0 -4.4201 0.2120
11 13 2 -1.2109 1.3623
11 13 4 -0.5103 2.2080
11 14 1 0.0374 0.9266
11 14 3 -1.9698 -1.4955
11 15 0 -0.5018 0.2432
11 15 2 -0.2403 2.4103
11 16 1 -0.0930 0.5798
12 0 0 -0.5889 -1.5921
12 0 2 -1.1767 -4.7093
12 1 1 3.1796 -1.1440
12 1 5 -0.0381 -0.9447
12 2 0 -1.2474 -0.7274
12 2 2 -0.5161 -3.9255
12 2 4 -0.5435 -3.4291
12 3 1 2.0695 -3.1853
12 3 3 -1.9628 -0.3088
12 3 5 0.3660 -0.7032
12 4 0 -2.5138 0.2143
12 4 2 0.6263 -1.8782
12 4 4 -0.6489 -3.8777
12 5 1 1.0104 -5.1783
12 5 3 1.8161 0.1926
12 5 5 0.2960 -0.5653
12 6 0 -2.4980 0.3288
12 6 2 1.0745 0.6038
12 6 4 -0.5336 -4.3569
12 7 1 0.7925 -5.3348
12 7 3 3.7074 0.1085
12 7 5 -0.6199 -0.5230
12 8 0 0.1790 -0.0707
12 8 2 1.0063 1.9171
12 8 4 -0.1460 -4.3368
12 9 1 1.0086 -3.8395
12 9 3 2.8669 0.0861
12 10 0 3.8940 -0.2321
12 10 2 1.0547 0.9408
12 10 4 0.2340 -3.3750
12 11 1 1.0863 -2.2755
12 11 3 0.8933 0.5368
12 12 0 4.8670 -0.1049
12 12 2 0.9344 -1.4139
12 13 1 0.9892 -1.5977
12 13 3 -0.1566 0.8857
12 14 0 1.8524 -0.1334
12 14 2 0.3137 -2.8082
12 15 1 0.6746 -1.2252
13 0 1 -5.3902 1.1228
13 0 5 1.1167 0.6077
13 1 0 -0.8258 1.3697
13 1 2 0.5397 3.7983
13 1 4 1.2178 3.2689
13 2 1 -3.8337 2.6978
13 2 3 1.6511 -0.2699
13 2 5 0.8402 0.5309
13 3 0 -0.9881 0.4521
13 3 2 -0.3815 2.2977
13 3 4 0.1793 2.4992
13 4 1 -1.0345 5.7641
13 4 3 0.1477 -0.4339
13 4 5 0.2599 0.2887
13 5 0 -1.0771 -0.1322
13 5 2 -0.5557 0.6117
13 5 4 -0.4436 2.0383
13 6 1 -0.0272 7.4123
13 6 3 -1.5196 -0.5974
13 7 0 -1.7465 -0.0788
13 7 2 0.3593 -0.0775
13 7 4 0.0597 2.2303
13 8 1 -1.0349 6.4830
13 8 3 -1.9015 -0.5946
13 9 0 -3.4646 0.0815
13 9 2 0.8470 0.3991
13 9 4 0.7435 2.1121
13 10 1 -1.9943 4.3163
13 10 3 -0.6312 -0.4068
13 11 0 -4.5566 -0.0403
13 11 2 0.3057 1.3916
13 12 1 -1.8315 2.7102
13 13 0 -2.9140 -0.1851
13 13 2 -0.0919 2.0256
14 0 0 2.8958 -1.0882
14 0 2 -2.0534 -2.7407
14 0 4 -1.9635 -1.5549
14 1 1 5.7070 -3.1683
14 1 3 -0.9654 1.1146
14 2 0 2.7963 -0.6227
14 2 2 -0.7017 -2.1723
14 2 4 -0.8217 -0.9798
14 3 1 2.1372 -4.3379
14 3 3 -1.3254 0.7084
14 4 0 2.1436 -0.0033
14 4 2 1.4256 -1.2301
14 4 4 0.9973 -0.1408
14 5 1 -0.7877 -5.2275
14 5 3 -0.9822 0.4918
14 6 0 1.1094 0.2920
14 6 2 1.5878 -0.9694
14 6 4 1.1227 -0.2082
14 7 1 -0.5145 -4.7803
14 7 3 0.0083 0.6091
14 8 0 1.0778 0.2416
14 8 2 0.2084 -1.2352
14 9 1 1.0677 -3.5373
14 9 3 0.3356 0.5466
14 10 0 2.2968 0.1744
14 10 2 -0.5196 -1.1921
14 11 1 1.4106 -2.6400
14 12 0 2.6941 0.2472
15 0 3 0.6385 -1.2396
15 1 0 -1.9111 -0.1385
15 1 2 2.3604 1.4225
15 1 4 1.9460 -0.5476
15 2 1 -3.9762 2.6250
15 2 3 1.1624 -0.9050
15 3 0 -0.9286 -0.2516
15 3 2 -0.8722 1.0515
15 4 1 0.2802 1.7964
15 4 3 1.7472 -0.3807
15 5 0 0.9807 -0.4396
15 5 2 -3.3861 0.8964
15 6 1 1.9818 0.7643
15 6 3 1.1379 -0.3384
15 7 0 2.3659 -0.5202
15 7 2 -2.8546 0.9860
15 8 1 0.9247 0.1916
15 9 0 1.5839 -0.3729
15 10 1 0.0280 0.5393
16 0 0 -1.8041 1.1258
16 0 2 -1.8644 0.0116
16 1 1 4.4284 -0.0893
16 1 3 -0.1019 0.2542
16 2 0 -1.8860 0.7558
16 2 2 -0.1612 -0.0536
16 3 1 0.9481 0.6630
16 4 0 -2.5051 0.4053
16 4 2 2.7687 -0.1825
16 5 1 -1.9972 1.5503
16 6 0 -3.5587 0.3760
16 7 1 -2.1191 1.8783
16 8 0 -3.5739 0.3825
17 0 1 -2.6607 -2.0424
17 1 0 4.0353 -0.9842
17 2 1 -1.2184 -1.8431
17 3 0 2.7563 -0.2383
0 0 0 0.0 0.0
;
_iucr_refine_instructions_details
;
exp_15827.res created by SHELXL-2014/7
TITL exp_15827_a.res in Imm2
REM Old TITL exp_15827 in Immm
REM SHELXT solution in Imm2
REM R1 0.081, Rweak 0.030, Alpha 0.006, Orientation a'=b, b'=c, c'=a
REM Flack x = 0.044 ( 0.020 ) from Parsons' quotients
REM Formula found by SHELXT: C23 O40 Mo6
CELL 1.54184 15.0786 18.8242 7.2176 90 90 90
ZERR 2 0.001 0.001 0.0005 0 0 0
LATT -2
SYMM -X,-Y,+Z
SYMM +X,-Y,+Z
SYMM -X,+Y,+Z
SFAC C H Mo Na O
UNIT 32 24 12 12 64
DELU 0.02 0.01 O2 C2 Mo2 O1
DELU 0.01 0.005 O5 C4 O4 C4
SIMU 0.005 0.01 3.8 $C
SIMU 0.005 0.01 3.8 $O
L.S. 20
PLAN 1
TEMP -100.15
FREE Na1 C2
BOND $H
list 4
ABIN
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM
REM
REM
WGHT 0.116300 15.247900
BASF 0.03403
FVAR 0.25437
MO1 3 0.415211 0.500000 0.441321 10.50000 0.02474 0.02144 =
0.03688 0.00000 0.00323 0.00000
MO2 3 0.276710 0.431033 0.777583 11.00000 0.04192 0.03704 =
0.03467 0.00260 0.00271 -0.00651
O1 5 0.309886 0.426647 0.480450 11.00000 0.03425 0.03353 =
0.05167 -0.00321 -0.00097 -0.00302
O10 5 0.500000 0.574226 0.492506 10.50000 0.03476 0.02194 =
0.05038 -0.00219 0.00000 0.00000
O9 5 0.402234 0.500000 0.205823 10.50000 0.04000 0.01707 =
0.05532 0.00000 -0.00505 0.00000
O7 5 0.376225 0.500000 0.751301 10.50000 0.03712 0.03031 =
0.04843 0.00000 -0.00076 0.00000
O2 5 0.366884 0.346244 0.741444 11.00000 0.03878 0.03454 =
0.05312 -0.00192 0.00001 -0.00327
O5 5 0.099579 0.287494 0.528634 11.00000 0.03321 0.05225 =
0.06422 -0.00909 -0.00012 -0.00693
O8 5 0.188967 0.500000 0.712941 10.50000 0.03789 0.03847 =
0.05120 0.00000 0.00115 0.00000
O3 5 0.405851 0.259001 0.549198 11.00000 0.03807 0.03785 =
0.05878 -0.00170 -0.00019 0.00369
O4 5 0.183829 0.357495 0.690666 11.00000 0.04044 0.04157 =
0.05502 -0.00360 0.00141 -0.00574
O6 5 0.268849 0.412164 1.002929 11.00000 0.05377 0.04245 =
0.05212 0.00116 0.00422 -0.00935
C1 1 0.323186 0.353350 0.418307 11.00000 0.02626 0.03260 =
0.04801 0.00348 0.00113 -0.00622
AFIX 13
H1 2 0.360660 0.351208 0.304131 11.00000 -1.20000
AFIX 0
C3 1 0.233712 0.319045 0.387972 11.00000 0.03011 0.03040 =
0.04909 0.00013 -0.00045 -0.00783
AFIX 23
H3A 2 0.205843 0.342158 0.279386 11.00000 -1.20000
H3B 2 0.243898 0.268679 0.354716 11.00000 -1.20000
AFIX 0
C4 1 0.168532 0.320801 0.543335 11.00000 0.02939 0.03467 =
0.05068 0.00124 0.00052 -0.00591
C2 1 0.368987 0.315061 0.585690 11.00000 0.02917 0.03149 =
0.05069 0.00064 -0.00180 -0.00595
NA1 4 0.500000 0.218668 0.781384 10.50000 0.04334 0.08371 =
0.09154 0.03998 0.00000 0.00000
NA2 4 0.000000 0.271763 0.788004 10.50000 0.04640 0.21156 =
0.05706 0.02539 0.00000 0.00000
NA3 4 0.500000 0.361712 0.062975 10.50000 0.09645 0.29248 =
0.33233 -0.20041 0.00000 0.00000
HKLF 4
REM exp_15827_a.res in Imm2
REM R1 = 0.0546 for 1405 Fo > 4sig(Fo) and 0.0559 for all 1451 data
REM 149 parameters refined using 153 restraints
END
WGHT 0.1160 15.5369
REM Highest difference peak 2.745, deepest hole -1.161, 1-sigma level 0.215
Q1 1 0.5000 0.5000 -0.0417 10.25000 0.05 2.75
REM The information below was added by Olex2.
REM
REM R1 = 0.0546 for 1405 Fo > 4sig(Fo) and 0.0559 for all 5531 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 2.75, deepest hole -1.16
REM Mean Shift 0.002, Max Shift 0.071.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0559
REM R1_gt = 0.0546
REM wR_ref = 0.1541
REM GOOF = 1.062
REM Shift_max = 0.071
REM Shift_mean = 0.002
REM Reflections_all = 5531
REM Reflections_gt = 1405
REM Parameters = n/a
REM Hole = -1.16
REM Peak = 2.75
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.97(6)
2 0.03(6)
#######################################################################
#
# 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_exp_17169
_database_code_depnum_ccdc_archive 'CCDC 1814438'
_audit_update_record
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_exp_17169
;
PROBLEM: D-H Without Acceptor O6 --H6A Please Check
RESPONSE: The unit cell of compound 3 includes a large region of disordered solvent water molecules which are of no interest. We employed a solvent mask to calculate the disraction contribution of the solvent molecules, and to produce a set of solvent-free disraction intensities. The Mask calculations showed a total solvent accessible area volume of 542.5 \%A3 and the residual electron density amounted to 168.7 electrons per unit cell, corresponding to 16 water molecules.
;
_vrf_PLAT420_exp_17169_2
;
PROBLEM: D-H Without Acceptor N2 --H2 Please Check
RESPONSE: The unit cell of compound 3 includes a large region of disordered solvent water molecules which are of no interest. We employed a solvent mask to calculate the disraction contribution of the solvent molecules, and to produce a set of solvent-free disraction intensities. The Mask calculations showed a total solvent accessible area volume of 542.5 \%A3 and the residual electron density amounted to 168.7 electrons per unit cell, corresponding to 16 water molecules.
;
# Added during the CSD deposition process: Friday 13 April 2018 02:14 PM
# end Validation Reply Form
_audit_creation_date 2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H50 Mo6 N20 O16'
_chemical_formula_sum 'C36 H50 Mo6 N20 O16'
_chemical_formula_weight 1594.60
_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'
Mo Mo -1.6832 0.6857 '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'
_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 triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.6194(5)
_cell_length_b 11.9177(5)
_cell_length_c 14.7094(10)
_cell_angle_alpha 90.197(4)
_cell_angle_beta 106.313(5)
_cell_angle_gamma 110.829(4)
_cell_volume 1658.78(16)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 2311
_cell_measurement_temperature 173
_cell_measurement_theta_max 25.5550
_cell_measurement_theta_min 2.9070
_shelx_estimated_absorpt_T_max 0.955
_shelx_estimated_absorpt_T_min 0.800
_exptl_absorpt_coefficient_mu 1.167
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.98843
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.596
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 786
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.04
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0453
_diffrn_reflns_av_unetI/netI 0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 11292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 25.000
_diffrn_reflns_theta_min 2.152
_diffrn_ambient_temperature 173
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 7.00 73.00 1.00 26.00 -- 24.10 57.00 -60.00 66
2 \w 51.00 81.00 1.00 26.00 -- 24.10-129.00 119.00 30
3 \w 68.00 95.00 1.00 26.00 -- 24.10-143.00 -51.00 27
4 \w -73.00 -44.00 1.00 26.00 -- -22.85-178.00 60.00 29
5 \w -95.00 -35.00 1.00 26.00 -- -22.85-178.00 90.00 60
6 \w -96.00 7.00 1.00 26.00 -- -22.85 -38.00 -60.00 103
7 \w -96.00 8.00 1.00 26.00 -- -22.85 -38.00 30.00 104
8 \w -104.00 -78.00 1.00 26.00 -- -22.85 178.00-180.00 26
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0088040000
_diffrn_orient_matrix_UB_12 0.0032397000
_diffrn_orient_matrix_UB_13 -0.0460913000
_diffrn_orient_matrix_UB_21 0.0740253000
_diffrn_orient_matrix_UB_22 0.0171863000
_diffrn_orient_matrix_UB_23 0.0206530000
_diffrn_orient_matrix_UB_31 -0.0078557000
_diffrn_orient_matrix_UB_32 -0.0616733000
_diffrn_orient_matrix_UB_33 -0.0027214000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4536
_reflns_number_total 5853
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 27.42
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_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 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 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 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.153
_refine_diff_density_min -1.031
_refine_diff_density_rms 0.121
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 364
_refine_ls_number_reflns 5853
_refine_ls_number_restraints 419
_refine_ls_R_factor_all 0.0689
_refine_ls_R_factor_gt 0.0520
_refine_ls_restrained_S_all 1.067
_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^)+(0.0493P)^2^+0.3511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1138
_refine_ls_wR_factor_ref 0.1199
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
N10-H10A
0.88 with sigma of 0.01
O6-H6A
0.85 with sigma of 0.01
C2-C1
1.5 with sigma of 0.01
3. Rigid bond restraints
C1, C3A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
O6, C1, Mo3, N7
with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.0025
Mo3, O3
with sigma for 1-2 distances of 0.00125 and sigma for 1-3 distances of 0.000625
C18, C17, C17, N10, N10, C16, C15, C14, C14, N8, N8, C13, C2, O7, C2, O8, C1,
C2
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C18 \\sim C17 \\sim C17 \\sim N10 \\sim N10 \\sim C16 \\sim C15 \\sim C14 \\sim
C14 \\sim N8 \\sim N8 \\sim C13 \\sim C2 \\sim O7 \\sim C2 \\sim O8 \\sim C1
\\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C7 \\sim C10 \\sim C4 \\sim C9 \\sim C12 \\sim C11 \\sim C2 \\sim C8 \\sim C6
\\sim C16 \\sim C15 \\sim C18 \\sim C5 \\sim C13 \\sim C17 \\sim C1 \\sim C14
\\sim C3 \\sim C3A: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.02
N3 \\sim N5 \\sim N1 \\sim N4 \\sim N9 \\sim N6 \\sim N7 \\sim N2 \\sim N8
\\sim N10: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01
O2 \\sim O5 \\sim O1 \\sim O3 \\sim O4 \\sim O7 \\sim O8 \\sim O6: within 3.8A
with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.01
Uanis(N8) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
Sof(H1B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
Sof(H1A)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
6.a Riding coordinates:
C3A(H6A)
6.b Ternary CH refined with riding coordinates:
C1(H1A), C1(H1B)
6.c Aromatic/amide H refined with riding coordinates:
N4(H4), N6(H6), C7(H7), N2(H2), C10(H10), C4(H4A), C9(H9), C12(H12), C11(H11),
C8(H8), C6(H6B), C16(H16), C15(H15), C18(H18), C5(H5), C13(H13), C17(H17),
N8(H8A), N10(H10A), C14(H14)
6.d Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC)
;
_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
Mo1 Mo 0.37482(6) 0.58778(4) 0.55856(4) 0.02377(16) Uani 1 1 d . . . . .
Mo2 Mo 0.62358(6) 0.61897(4) 0.41397(4) 0.02320(15) Uani 1 1 d . . . . .
Mo3 Mo 0.36465(6) 0.50881(5) 0.71864(4) 0.02708(16) Uani 1 1 d . U . . .
O2 O 0.7524(4) 0.5707(3) 0.5088(3) 0.0268(8) Uani 1 1 d . U . . .
O5 O 0.4929(4) 0.6263(3) 0.4772(3) 0.0274(8) Uani 1 1 d . U . . .
O1 O 0.5234(4) 0.5432(3) 0.6568(3) 0.0301(7) Uani 1 1 d . U . . .
O3 O 0.2438(4) 0.3465(3) 0.6650(3) 0.0311(7) Uani 1 1 d . U . . .
O4 O 0.2596(4) 0.5935(3) 0.6439(3) 0.0310(8) Uani 1 1 d . U . . .
O7 O 0.4836(5) 0.2991(4) 0.7014(3) 0.0338(8) Uani 1 1 d . U . . .
O8 O 0.4839(5) 0.4233(4) 0.8187(3) 0.0367(8) Uani 1 1 d . U . . .
N3 N 0.2311(5) 0.6559(4) 0.4570(4) 0.0254(11) Uani 1 1 d . U . . .
N5 N 0.7528(6) 0.8050(4) 0.4831(4) 0.0305(11) Uani 1 1 d . U . . .
N1 N 0.5011(6) 0.7794(4) 0.6230(4) 0.0311(10) Uani 1 1 d . U . . .
N4 N 0.0375(5) 0.6830(4) 0.3815(4) 0.0333(12) Uani 1 1 d . U . . .
H4 H -0.0480 0.6843 0.3687 0.040 Uiso 1 1 calc R . . . .
N9 N 0.2306(6) 0.4851(5) 0.8115(4) 0.0417(13) Uani 1 1 d . U . . .
N6 N 0.9164(6) 0.9611(4) 0.5767(4) 0.0389(13) Uani 1 1 d . U . . .
H6 H 0.9950 1.0066 0.6201 0.047 Uiso 1 1 calc R . . . .
N7 N 0.5112(6) 0.6641(5) 0.8246(4) 0.0386(12) Uani 1 1 d . U . . .
C7 C 0.1022(7) 0.6446(5) 0.4571(5) 0.0297(14) Uani 1 1 d . U . . .
H7 H 0.0619 0.6126 0.5059 0.036 Uiso 1 1 calc R . . . .
N2 N 0.6788(7) 0.9363(5) 0.7037(4) 0.0426(13) Uani 1 1 d . U . . .
H2 H 0.7649 0.9819 0.7383 0.051 Uiso 1 1 calc R . . . .
C10 C 0.8787(7) 0.8452(5) 0.5501(5) 0.0328(15) Uani 1 1 d . U . . .
H10 H 0.9328 0.7974 0.5748 0.039 Uiso 1 1 calc R . . . .
C4 C 0.6358(7) 0.8201(5) 0.6729(5) 0.0345(14) Uani 1 1 d . U . . .
H4A H 0.6935 0.7733 0.6850 0.041 Uiso 1 1 calc R . . . .
C9 C 0.2456(7) 0.7036(5) 0.3744(5) 0.0333(15) Uani 1 1 d . U . . .
H9 H 0.3274 0.7218 0.3541 0.040 Uiso 1 1 calc R . . . .
C12 C 0.7127(7) 0.9031(6) 0.4684(5) 0.0395(16) Uani 1 1 d . U . . .
H12 H 0.6277 0.9032 0.4247 0.047 Uiso 1 1 calc R . . . .
O6 O 0.6092(7) 0.1837(5) 0.8265(4) 0.0706(14) Uani 1 1 d D U . . .
C11 C 0.8144(7) 0.9977(6) 0.5263(5) 0.0389(16) Uani 1 1 d . U . . .
H11 H 0.8147 1.0773 0.5311 0.047 Uiso 1 1 calc R . . . .
C2 C 0.5277(8) 0.3420(5) 0.7926(5) 0.0388(16) Uani 1 1 d D U . . .
C8 C 0.1261(7) 0.7213(6) 0.3255(5) 0.0373(16) Uani 1 1 d . U . . .
H8 H 0.1077 0.7529 0.2661 0.045 Uiso 1 1 calc R . . . .
C6 C 0.4604(8) 0.8758(6) 0.6236(6) 0.0440(17) Uani 1 1 d . U . . .
H6B H 0.3681 0.8742 0.5932 0.053 Uiso 1 1 calc R . . . .
C16 C 0.1411(9) 0.5386(7) 0.8122(6) 0.0572(19) Uani 1 1 d . U . . .
H16 H 0.1238 0.5955 0.7703 0.069 Uiso 1 1 calc R . . . .
C15 C 0.6493(8) 0.6880(6) 0.8734(6) 0.0501(18) Uani 1 1 d . U . . .
H15 H 0.7000 0.6377 0.8692 0.060 Uiso 1 1 calc R . . . .
C18 C 0.2191(10) 0.4114(8) 0.8793(6) 0.061(2) Uani 1 1 d . U . . .
H18 H 0.2702 0.3595 0.8955 0.074 Uiso 1 1 calc R . . . .
C5 C 0.5704(8) 0.9728(6) 0.6735(6) 0.0472(17) Uani 1 1 d . U . . .
H5 H 0.5711 1.0516 0.6851 0.057 Uiso 1 1 calc R . . . .
C13 C 0.4826(9) 0.7582(6) 0.8507(6) 0.0543(18) Uani 1 1 d . U . . .
H13 H 0.3935 0.7663 0.8290 0.065 Uiso 1 1 calc R . . . .
C17 C 0.1270(10) 0.4202(8) 0.9212(6) 0.067(2) Uani 1 1 d . U . . .
H17 H 0.1007 0.3766 0.9711 0.080 Uiso 1 1 calc R . . . .
N8 N 0.6011(7) 0.8402(6) 0.9132(5) 0.0598(15) Uani 1 1 d . U . . .
H8A H 0.6093 0.9103 0.9388 0.072 Uiso 1 1 calc R . . . .
N10 N 0.0783(8) 0.5024(6) 0.8792(5) 0.0673(17) Uani 1 1 d D U . . .
H10A H 0.0167 0.5276 0.8932 0.081 Uiso 1 1 calc DR . . . .
C1 C 0.6053(10) 0.2900(7) 0.8642(6) 0.061(2) Uani 1 1 d D U . . .
H1A H 0.7051 0.3484 0.8793 0.073 Uiso 0.496(14) 1 calc R . P A 1
H1B H 0.5662 0.2755 0.9194 0.073 Uiso 0.504(14) 1 calc R . P A 2
C14 C 0.7024(9) 0.7947(7) 0.9285(6) 0.061(2) Uani 1 1 d . U . . .
H14 H 0.7956 0.8312 0.9708 0.073 Uiso 1 1 calc R . . . .
C3 C 0.581(2) 0.2836(15) 0.9472(13) 0.065(4) Uani 0.496(14) 1 d . U P A 1
H3A H 0.4921 0.2168 0.9418 0.098 Uiso 0.496(14) 1 calc GR . P A 1
H3B H 0.5759 0.3596 0.9675 0.098 Uiso 0.496(14) 1 calc GR . P A 1
H3C H 0.6587 0.2695 0.9944 0.098 Uiso 0.496(14) 1 calc GR . P A 1
C3A C 0.742(2) 0.3780(12) 0.8913(13) 0.082(5) Uani 0.504(14) 1 d . U P A 2
H3AA H 0.8042 0.3507 0.9409 0.123 Uiso 0.504(14) 1 calc GR . P A 2
H3AB H 0.7401 0.4537 0.9161 0.123 Uiso 0.504(14) 1 calc GR . P A 2
H3AC H 0.7771 0.3915 0.8358 0.123 Uiso 0.504(14) 1 calc GR . P A 2
H6A H 0.6039 0.1140 0.8518 0.098 Uiso 1 1 d DR . . . .
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
Mo1 0.0199(3) 0.0184(3) 0.0329(4) 0.0042(2) 0.0069(2) 0.0078(2)
Mo2 0.0205(3) 0.0185(3) 0.0308(3) 0.0050(2) 0.0078(2) 0.0075(2)
Mo3 0.0267(3) 0.0232(3) 0.0322(4) 0.0044(2) 0.0089(3) 0.0104(2)
O2 0.0273(16) 0.0228(15) 0.0344(17) 0.0066(13) 0.0126(14) 0.0113(14)
O5 0.0286(16) 0.0230(15) 0.0332(17) 0.0056(13) 0.0113(14) 0.0110(14)
O1 0.0294(13) 0.0266(11) 0.0364(14) 0.0066(11) 0.0100(11) 0.0128(11)
O3 0.0297(14) 0.0271(11) 0.0377(15) 0.0057(11) 0.0087(12) 0.0129(11)
O4 0.0296(16) 0.0272(15) 0.0388(18) 0.0054(14) 0.0116(14) 0.0125(14)
O7 0.0330(15) 0.0314(14) 0.0391(16) 0.0068(12) 0.0092(13) 0.0157(13)
O8 0.0351(15) 0.0327(14) 0.0401(16) 0.0078(12) 0.0066(13) 0.0139(13)
N3 0.027(2) 0.019(2) 0.035(3) 0.0061(18) 0.013(2) 0.0114(19)
N5 0.035(2) 0.021(2) 0.038(3) 0.0038(19) 0.015(2) 0.010(2)
N1 0.033(2) 0.0245(19) 0.039(2) 0.0068(17) 0.0133(19) 0.0130(18)
N4 0.024(3) 0.030(3) 0.046(3) 0.005(2) 0.005(2) 0.014(2)
N9 0.047(3) 0.042(3) 0.044(3) 0.009(2) 0.021(2) 0.019(2)
N6 0.040(3) 0.023(2) 0.047(3) -0.001(2) 0.012(2) 0.005(2)
N7 0.044(2) 0.031(2) 0.041(3) 0.0050(19) 0.011(2) 0.016(2)
C7 0.024(3) 0.029(3) 0.036(4) 0.009(3) 0.009(3) 0.010(3)
N2 0.045(2) 0.030(2) 0.046(3) 0.003(2) 0.010(2) 0.007(2)
C10 0.030(3) 0.025(3) 0.044(4) 0.006(3) 0.015(3) 0.007(3)
C4 0.035(3) 0.025(2) 0.043(3) 0.002(2) 0.012(2) 0.010(2)
C9 0.028(3) 0.032(3) 0.044(4) 0.008(3) 0.017(3) 0.011(3)
C12 0.036(3) 0.036(3) 0.049(4) 0.011(3) 0.012(3) 0.016(3)
O6 0.075(3) 0.057(2) 0.065(3) 0.003(2) -0.004(3) 0.025(2)
C11 0.042(3) 0.024(3) 0.046(4) 0.006(3) 0.008(3) 0.011(3)
C2 0.073(4) 0.019(3) 0.036(4) 0.004(3) 0.037(3) 0.015(3)
C8 0.028(3) 0.037(3) 0.049(4) 0.009(3) 0.012(3) 0.014(3)
C6 0.041(4) 0.030(3) 0.060(4) -0.002(3) 0.008(3) 0.017(3)
C16 0.078(4) 0.059(4) 0.051(4) 0.017(3) 0.036(4) 0.032(4)
C15 0.044(4) 0.040(3) 0.052(4) 0.001(3) -0.004(3) 0.013(3)
C18 0.088(5) 0.082(5) 0.042(4) 0.022(4) 0.038(4) 0.049(4)
C5 0.046(3) 0.031(3) 0.062(4) -0.006(3) 0.007(3) 0.018(3)
C13 0.054(3) 0.041(3) 0.056(4) -0.004(3) 0.003(3) 0.015(3)
C17 0.089(5) 0.091(5) 0.055(5) 0.030(4) 0.049(4) 0.052(4)
N8 0.065(3) 0.046(2) 0.057(3) -0.003(2) 0.007(2) 0.015(2)
N10 0.070(3) 0.073(3) 0.067(3) 0.010(3) 0.029(3) 0.029(3)
C1 0.076(5) 0.057(4) 0.050(5) -0.006(3) 0.013(4) 0.029(4)
C14 0.051(4) 0.045(4) 0.055(4) -0.003(3) -0.015(4) 0.004(3)
C3 0.073(7) 0.070(7) 0.067(7) 0.010(6) 0.022(6) 0.043(6)
C3A 0.077(7) 0.076(7) 0.082(8) 0.011(6) 0.011(6) 0.027(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
Mo1 Mo2 2.5034(7) 2_666 ?
Mo1 Mo3 2.5550(8) . ?
Mo1 O2 1.948(4) 2_666 ?
Mo1 O5 1.911(4) . ?
Mo1 O1 2.044(4) . ?
Mo1 O4 2.000(4) . ?
Mo1 N3 2.198(5) . ?
Mo1 N1 2.237(5) . ?
Mo2 Mo1 2.5035(7) 2_666 ?
Mo2 Mo3 2.5282(8) 2_666 ?
Mo2 O2 1.908(4) . ?
Mo2 O5 1.900(4) . ?
Mo2 O1 2.045(4) 2_666 ?
Mo2 O3 2.003(4) 2_666 ?
Mo2 O7 2.201(4) 2_666 ?
Mo2 N5 2.207(5) . ?
Mo3 Mo2 2.5282(8) 2_666 ?
Mo3 O1 2.052(4) . ?
Mo3 O3 1.915(4) . ?
Mo3 O4 1.895(4) . ?
Mo3 O8 2.165(4) . ?
Mo3 N9 2.186(6) . ?
Mo3 N7 2.202(6) . ?
O2 Mo1 1.948(4) 2_666 ?
O1 Mo2 2.045(4) 2_666 ?
O3 Mo2 2.003(4) 2_666 ?
O7 Mo2 2.201(4) 2_666 ?
O7 C2 1.324(7) . ?
O8 C2 1.312(7) . ?
N3 C7 1.327(8) . ?
N3 C9 1.368(8) . ?
N5 C10 1.338(8) . ?
N5 C12 1.377(8) . ?
N1 C4 1.317(8) . ?
N1 C6 1.364(8) . ?
N4 H4 0.8800 . ?
N4 C7 1.309(8) . ?
N4 C8 1.381(8) . ?
N9 C16 1.322(9) . ?
N9 C18 1.334(9) . ?
N6 H6 0.8800 . ?
N6 C10 1.318(8) . ?
N6 C11 1.342(8) . ?
N7 C15 1.362(9) . ?
N7 C13 1.342(9) . ?
C7 H7 0.9500 . ?
N2 H2 0.8800 . ?
N2 C4 1.327(8) . ?
N2 C5 1.335(9) . ?
C10 H10 0.9500 . ?
C4 H4A 0.9500 . ?
C9 H9 0.9500 . ?
C9 C8 1.361(9) . ?
C12 H12 0.9500 . ?
C12 C11 1.332(9) . ?
O6 C1 1.399(9) . ?
O6 H6A 0.9008 . ?
C11 H11 0.9500 . ?
C2 C1 1.432(7) . ?
C8 H8 0.9500 . ?
C6 H6B 0.9500 . ?
C6 C5 1.339(9) . ?
C16 H16 0.9500 . ?
C16 N10 1.330(10) . ?
C15 H15 0.9500 . ?
C15 C14 1.348(10) . ?
C18 H18 0.9500 . ?
C18 C17 1.325(11) . ?
C5 H5 0.9500 . ?
C13 H13 0.9500 . ?
C13 N8 1.360(9) . ?
C17 H17 0.9500 . ?
C17 N10 1.340(10) . ?
N8 H8A 0.8800 . ?
N8 C14 1.334(10) . ?
N10 H10A 0.8800 . ?
C1 H1A 1.0000 . ?
C1 H1B 1.0000 . ?
C1 C3 1.312(18) . ?
C1 C3A 1.398(18) . ?
C14 H14 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Mo2 Mo1 Mo3 59.96(2) 2_666 . ?
O2 Mo1 Mo2 48.81(12) 2_666 2_666 ?
O2 Mo1 Mo3 90.66(12) 2_666 . ?
O2 Mo1 O1 100.99(16) 2_666 . ?
O2 Mo1 O4 95.37(17) 2_666 . ?
O2 Mo1 N3 84.98(17) 2_666 . ?
O2 Mo1 N1 172.39(18) 2_666 . ?
O5 Mo1 Mo2 97.75(11) . 2_666 ?
O5 Mo1 Mo3 141.51(13) . . ?
O5 Mo1 O2 96.55(17) . 2_666 ?
O5 Mo1 O1 89.97(17) . . ?
O5 Mo1 O4 164.95(16) . . ?
O5 Mo1 N3 87.90(18) . . ?
O5 Mo1 N1 83.51(18) . . ?
O1 Mo1 Mo2 52.27(11) . 2_666 ?
O1 Mo1 Mo3 51.56(12) . . ?
O1 Mo1 N3 173.86(17) . . ?
O1 Mo1 N1 86.62(18) . . ?
O4 Mo1 Mo2 97.01(11) . 2_666 ?
O4 Mo1 Mo3 47.25(12) . . ?
O4 Mo1 O1 96.75(17) . . ?
O4 Mo1 N3 84.01(18) . . ?
O4 Mo1 N1 83.46(18) . . ?
N3 Mo1 Mo2 133.76(13) . 2_666 ?
N3 Mo1 Mo3 130.47(13) . . ?
N3 Mo1 N1 87.42(19) . . ?
N1 Mo1 Mo2 138.77(14) . 2_666 ?
N1 Mo1 Mo3 94.00(14) . . ?
Mo1 Mo2 Mo3 61.03(2) 2_666 2_666 ?
O2 Mo2 Mo1 50.22(12) . 2_666 ?
O2 Mo2 Mo3 92.42(12) . 2_666 ?
O2 Mo2 O1 102.36(16) . 2_666 ?
O2 Mo2 O3 89.27(17) . 2_666 ?
O2 Mo2 O7 167.67(16) . 2_666 ?
O2 Mo2 N5 86.12(18) . . ?
O5 Mo2 Mo1 101.15(11) . 2_666 ?
O5 Mo2 Mo3 139.71(12) . 2_666 ?
O5 Mo2 O2 102.60(17) . . ?
O5 Mo2 O1 88.04(17) . 2_666 ?
O5 Mo2 O3 164.16(16) . 2_666 ?
O5 Mo2 O7 86.75(17) . 2_666 ?
O5 Mo2 N5 85.65(18) . . ?
O1 Mo2 Mo1 52.24(11) 2_666 2_666 ?
O1 Mo2 Mo3 52.03(12) 2_666 2_666 ?
O1 Mo2 O7 85.79(16) 2_666 2_666 ?
O1 Mo2 N5 170.38(18) 2_666 . ?
O3 Mo2 Mo1 94.50(11) 2_666 2_666 ?
O3 Mo2 Mo3 48.31(11) 2_666 2_666 ?
O3 Mo2 O1 99.74(17) 2_666 2_666 ?
O3 Mo2 O7 80.15(17) 2_666 2_666 ?
O3 Mo2 N5 84.73(18) 2_666 . ?
O7 Mo2 Mo1 136.42(11) 2_666 2_666 ?
O7 Mo2 Mo3 85.31(12) 2_666 2_666 ?
O7 Mo2 N5 86.60(18) 2_666 . ?
N5 Mo2 Mo1 136.33(14) . 2_666 ?
N5 Mo2 Mo3 133.04(14) . 2_666 ?
Mo2 Mo3 Mo1 59.01(2) 2_666 . ?
O1 Mo3 Mo1 51.27(12) . . ?
O1 Mo3 Mo2 51.77(11) . 2_666 ?
O1 Mo3 O8 84.52(17) . . ?
O1 Mo3 N9 168.4(2) . . ?
O1 Mo3 N7 86.3(2) . . ?
O3 Mo3 Mo1 95.10(13) . . ?
O3 Mo3 Mo2 51.35(13) . 2_666 ?
O3 Mo3 O1 102.50(17) . . ?
O3 Mo3 O8 84.34(17) . . ?
O3 Mo3 N9 84.9(2) . . ?
O3 Mo3 N7 160.37(19) . . ?
O4 Mo3 Mo1 50.81(13) . . ?
O4 Mo3 Mo2 99.04(13) . 2_666 ?
O4 Mo3 O1 99.90(17) . . ?
O4 Mo3 O3 99.66(18) . . ?
O4 Mo3 O8 173.18(18) . . ?
O4 Mo3 N9 87.5(2) . . ?
O4 Mo3 N7 95.98(19) . . ?
O8 Mo3 Mo1 134.72(13) . . ?
O8 Mo3 Mo2 87.77(12) . 2_666 ?
O8 Mo3 N9 87.4(2) . . ?
O8 Mo3 N7 79.03(18) . . ?
N9 Mo3 Mo1 137.80(16) . . ?
N9 Mo3 Mo2 136.23(15) . 2_666 ?
N9 Mo3 N7 84.0(2) . . ?
N7 Mo3 Mo1 104.00(15) . . ?
N7 Mo3 Mo2 137.23(16) . 2_666 ?
Mo2 O2 Mo1 80.97(16) . 2_666 ?
Mo2 O5 Mo1 160.4(2) . . ?
Mo1 O1 Mo2 75.49(15) . 2_666 ?
Mo1 O1 Mo3 77.17(15) . . ?
Mo2 O1 Mo3 76.20(14) 2_666 . ?
Mo3 O3 Mo2 80.34(15) . 2_666 ?
Mo3 O4 Mo1 81.94(16) . . ?
C2 O7 Mo2 123.7(4) . 2_666 ?
C2 O8 Mo3 123.4(4) . . ?
C7 N3 Mo1 126.3(4) . . ?
C7 N3 C9 105.1(5) . . ?
C9 N3 Mo1 128.1(4) . . ?
C10 N5 Mo2 128.5(4) . . ?
C10 N5 C12 106.1(5) . . ?
C12 N5 Mo2 125.3(5) . . ?
C4 N1 Mo1 124.4(4) . . ?
C4 N1 C6 105.5(6) . . ?
C6 N1 Mo1 130.0(5) . . ?
C7 N4 H4 125.7 . . ?
C7 N4 C8 108.5(6) . . ?
C8 N4 H4 125.7 . . ?
C16 N9 Mo3 128.0(5) . . ?
C16 N9 C18 104.3(7) . . ?
C18 N9 Mo3 127.6(5) . . ?
C10 N6 H6 125.9 . . ?
C10 N6 C11 108.2(6) . . ?
C11 N6 H6 125.9 . . ?
C15 N7 Mo3 127.9(5) . . ?
C13 N7 Mo3 126.0(5) . . ?
C13 N7 C15 106.0(6) . . ?
N3 C7 H7 124.2 . . ?
N4 C7 N3 111.6(6) . . ?
N4 C7 H7 124.2 . . ?
C4 N2 H2 125.5 . . ?
C4 N2 C5 109.0(6) . . ?
C5 N2 H2 125.5 . . ?
N5 C10 H10 125.2 . . ?
N6 C10 N5 109.7(6) . . ?
N6 C10 H10 125.2 . . ?
N1 C4 N2 109.9(6) . . ?
N1 C4 H4A 125.1 . . ?
N2 C4 H4A 125.1 . . ?
N3 C9 H9 124.9 . . ?
C8 C9 N3 110.2(6) . . ?
C8 C9 H9 124.9 . . ?
N5 C12 H12 126.1 . . ?
C11 C12 N5 107.8(6) . . ?
C11 C12 H12 126.1 . . ?
C1 O6 H6A 130.5 . . ?
N6 C11 H11 125.9 . . ?
C12 C11 N6 108.2(6) . . ?
C12 C11 H11 125.9 . . ?
O7 C2 C1 121.4(6) . . ?
O8 C2 O7 118.7(6) . . ?
O8 C2 C1 119.3(6) . . ?
N4 C8 H8 127.7 . . ?
C9 C8 N4 104.5(6) . . ?
C9 C8 H8 127.7 . . ?
N1 C6 H6B 125.2 . . ?
C5 C6 N1 109.7(6) . . ?
C5 C6 H6B 125.2 . . ?
N9 C16 H16 124.3 . . ?
N9 C16 N10 111.3(7) . . ?
N10 C16 H16 124.3 . . ?
N7 C15 H15 125.5 . . ?
C14 C15 N7 109.0(8) . . ?
C14 C15 H15 125.5 . . ?
N9 C18 H18 124.4 . . ?
C17 C18 N9 111.2(8) . . ?
C17 C18 H18 124.4 . . ?
N2 C5 C6 105.9(6) . . ?
N2 C5 H5 127.0 . . ?
C6 C5 H5 127.0 . . ?
N7 C13 H13 125.3 . . ?
N7 C13 N8 109.5(7) . . ?
N8 C13 H13 125.3 . . ?
C18 C17 H17 126.7 . . ?
C18 C17 N10 106.6(8) . . ?
N10 C17 H17 126.7 . . ?
C13 N8 H8A 126.3 . . ?
C14 N8 C13 107.4(6) . . ?
C14 N8 H8A 126.3 . . ?
C16 N10 C17 106.6(7) . . ?
C16 N10 H10A 126.7 . . ?
C17 N10 H10A 126.7 . . ?
O6 C1 C2 111.5(7) . . ?
O6 C1 H1A 103.6 . . ?
O6 C1 H1B 111.1 . . ?
O6 C1 C3A 108.7(10) . . ?
C2 C1 H1A 103.6 . . ?
C2 C1 H1B 111.1 . . ?
C3 C1 O6 114.2(10) . . ?
C3 C1 C2 118.1(11) . . ?
C3 C1 H1A 103.6 . . ?
C3A C1 C2 103.1(8) . . ?
C3A C1 H1B 111.1 . . ?
C15 C14 H14 126.0 . . ?
N8 C14 C15 108.0(7) . . ?
N8 C14 H14 126.0 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C3A H3AA 109.5 . . ?
C1 C3A H3AB 109.5 . . ?
C1 C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.449 0.000 0.000 542.5 168.7 16H2O
2 0.500 0.500 0.000 11.9 0.0 ?
_shelx_fab_file
;
-12 1 4 6.2930 -0.0442
-12 1 5 -0.6637 -0.0501
-12 1 6 -3.6597 0.0399
-12 1 7 -1.6549 0.0122
-12 2 2 0.7418 -0.1003
-12 2 3 -1.7470 -0.0345
-12 2 4 -0.0028 0.0507
-12 2 5 3.5875 -0.0108
-12 2 6 -5.5035 -0.0096
-12 2 7 -4.4542 0.0160
-12 2 8 9.9123 0.0149
-12 3 1 0.3830 -0.1357
-12 3 2 -5.2323 0.0956
-12 3 3 -4.1306 0.0487
-12 3 4 1.9578 -0.0833
-12 3 5 -2.5752 0.0147
-12 3 6 -3.5589 0.0003
-12 3 7 1.4099 0.0100
-12 3 8 8.1234 -0.0203
-12 3 9 7.0062 0.0103
-12 4 1 -2.4097 0.1156
-12 4 2 -0.9845 -0.0835
-12 4 3 1.7053 -0.0354
-12 4 4 -3.2653 0.0894
-12 4 5 1.0289 -0.0750
-12 4 6 5.4737 0.0189
-12 4 7 -0.4137 0.0080
-12 4 8 1.0166 -0.0208
-12 4 9 1.1951 0.0142
-12 5 1 0.1039 -0.0526
-12 5 2 -1.2898 0.0147
-12 5 3 1.0899 0.0030
-12 5 4 1.9563 -0.0704
-12 5 5 3.2921 0.0724
-12 5 6 1.1133 -0.0135
-12 5 7 0.1271 -0.0312
-12 5 8 0.0415 0.0274
-12 5 9 0.0520 -0.0371
-12 6 1 -1.4069 0.0109
-12 6 2 -3.0369 -0.0224
-12 6 3 1.7060 -0.0173
-12 6 4 2.5366 0.0566
-12 6 5 -0.5645 -0.0561
-12 6 6 0.5069 -0.0074
-12 6 7 1.7775 0.0385
-12 6 8 -2.5335 -0.0535
-12 6 9 -1.7185 0.0099
-12 7 1 3.4208 0.0783
-12 7 2 1.3905 0.0265
-12 7 3 -1.4088 0.0148
-12 7 4 0.6547 -0.0358
-12 7 5 -0.8717 0.0136
-12 7 6 -2.8616 0.0324
-12 7 7 -4.2122 0.0118
-12 7 8 -2.1507 0.0166
-12 8 1 8.6719 -0.0444
-12 8 2 -1.1786 -0.0268
-12 8 3 -3.7547 -0.0002
-12 8 4 2.8081 0.0400
-12 8 5 -1.1869 0.0475
-12 8 6 -9.5247 -0.0458
-12 8 7 -1.4860 0.0042
-11 -2 4 4.2846 0.0795
-11 -2 5 0.8840 -0.0377
-11 -2 6 0.8766 -0.0177
-11 -1 1 0.9801 0.0199
-11 -1 2 2.6933 0.0001
-11 -1 3 3.3987 -0.0194
-11 -1 4 1.6014 -0.0663
-11 -1 5 0.0447 0.0569
-11 -1 6 -1.9334 0.0403
-11 -1 7 0.1024 -0.0421
-11 -1 8 5.3219 -0.0537
-11 -1 9 1.4320 0.0219
-11 0 1 0.3485 -0.0739
-11 0 2 0.9201 -0.0606
-11 0 3 0.6264 0.0746
-11 0 4 1.9118 0.0062
-11 0 5 0.1515 -0.0494
-11 0 6 -3.4263 -0.0332
-11 0 7 0.3429 0.0121
-11 0 8 1.1281 0.0258
-11 0 9 0.8389 -0.0324
-11 0 10 0.9579 -0.0601
-11 1 1 -0.6228 0.0533
-11 1 2 1.6118 0.0438
-11 1 3 3.4687 -0.0870
-11 1 4 -0.6130 0.0121
-11 1 5 -0.7167 0.0338
-11 1 6 0.0004 0.0204
-11 1 7 -5.7506 -0.0135
-11 1 8 -2.1820 -0.0431
-11 1 9 4.3615 0.0295
-11 1 10 0.8972 0.0403
-11 1 11 -2.7239 -0.0421
-11 2 1 1.1460 -0.0736
-11 2 2 3.2235 -0.0458
-11 2 3 -1.3658 0.0930
-11 2 4 -2.4979 -0.0254
-11 2 5 1.0048 -0.0140
-11 2 6 -3.9601 0.0341
-11 2 7 -7.4970 -0.0294
-11 2 8 -2.3320 0.0076
-11 2 9 5.7088 -0.0142
-11 2 10 2.0601 -0.0065
-11 2 11 -4.3813 0.0261
-11 2 12 -0.3064 0.0101
-11 3 1 -2.0773 0.1111
-11 3 2 1.5296 0.0307
-11 3 3 1.7524 -0.1048
-11 3 4 -3.8785 0.0371
-11 3 5 -7.3973 0.0138
-11 3 6 -0.8742 -0.0638
-11 3 7 -2.8973 0.0585
-11 3 8 -3.4202 -0.0373
-11 3 9 2.9297 -0.0435
-11 3 10 0.2572 0.0481
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8 3 1 2.7659 -0.0098
8 3 2 4.1780 -0.0157
8 3 3 1.9171 0.0538
8 3 4 -3.5732 -0.0622
8 3 5 -1.2991 0.0111
8 3 6 4.7621 0.0649
8 4 0 0.3476 -0.0498
8 4 1 -0.2376 0.0330
8 4 2 0.5220 -0.0298
8 4 3 3.2343 -0.0361
8 4 4 0.3238 0.0580
8 4 5 -0.8807 0.0638
8 5 0 0.7420 0.0612
8 5 1 -0.6503 -0.0023
8 5 2 -2.4439 -0.0485
8 5 3 2.9268 0.0051
8 6 0 3.7764 0.0454
8 6 1 -1.5889 -0.0049
9 -12 0 5.7030 0.0007
9 -12 1 2.6359 0.0812
9 -12 2 -7.8403 -0.0084
9 -11 0 5.2306 0.0562
9 -11 1 -3.0486 -0.0910
9 -11 2 -2.9124 -0.0026
9 -11 3 0.9161 -0.0057
9 -11 4 0.3576 -0.0342
9 -10 0 3.0017 -0.0474
9 -10 1 4.2652 0.0510
9 -10 2 -0.1349 -0.0220
9 -10 3 -2.3068 -0.0380
9 -10 4 -1.0910 0.0278
9 -10 5 -8.1002 0.0466
9 -9 0 2.8060 0.0666
9 -9 1 5.9617 -0.0555
9 -9 2 -4.2122 -0.0209
9 -9 3 -1.2532 0.0349
9 -9 4 0.9660 -0.0153
9 -9 5 -0.7902 -0.0115
9 -9 6 0.5705 0.0187
9 -8 0 1.1976 -0.0422
9 -8 1 5.5733 0.0425
9 -8 2 0.9703 -0.0008
9 -8 3 -1.3297 -0.0538
9 -8 4 3.9200 -0.0075
9 -8 5 4.4889 0.0297
9 -8 6 -1.7247 0.0106
9 -8 7 2.6208 -0.0493
9 -7 0 0.5181 0.0698
9 -7 1 0.8948 -0.0359
9 -7 2 0.7742 -0.0093
9 -7 3 0.0956 0.0640
9 -7 4 -1.4922 -0.0061
9 -7 5 -2.5537 -0.0256
9 -7 6 2.4330 -0.0135
9 -7 7 4.2308 0.0397
9 -6 0 -4.6771 -0.0432
9 -6 1 -4.9430 0.0312
9 -6 2 1.9030 0.0228
9 -6 3 -1.2154 -0.0313
9 -6 4 -5.0839 0.0239
9 -6 5 1.5688 -0.0148
9 -6 6 0.7924 0.0486
9 -6 7 -0.4706 -0.0588
9 -6 8 5.1473 0.0108
9 -5 0 -1.6315 0.0395
9 -5 1 -1.6946 -0.0634
9 -5 2 -0.5779 -0.0339
9 -5 3 -0.8575 0.0546
9 -5 4 0.6070 -0.0328
9 -5 5 -3.6534 0.0149
9 -5 6 -2.9858 -0.0155
9 -5 7 1.8048 0.0478
9 -5 8 2.5796 0.0234
9 -4 0 0.7900 0.0000
9 -4 1 -2.7478 0.0960
9 -4 2 -2.1856 -0.0225
9 -4 3 0.5671 -0.0629
9 -4 4 -0.5320 0.0768
9 -4 5 -3.3285 -0.0272
9 -4 6 -0.1789 -0.0032
9 -4 7 -0.4742 0.0395
9 -4 8 1.2091 -0.0430
9 -3 0 -3.8422 0.0106
9 -3 1 -1.1440 -0.1026
9 -3 2 -1.8289 0.0739
9 -3 3 -3.2777 0.0546
9 -3 4 2.3938 -0.0749
9 -3 5 3.5747 0.0355
9 -3 6 -0.4185 0.0332
9 -3 7 -1.9044 -0.0308
9 -3 8 -1.5183 0.1103
9 -2 0 1.2805 -0.0542
9 -2 1 -2.1450 0.1267
9 -2 2 -6.4538 -0.0500
9 -2 3 1.0131 -0.0591
9 -2 4 5.7349 0.0840
9 -2 5 -0.4505 0.0020
9 -2 6 -0.6155 -0.0233
9 -2 7 2.5587 0.0362
9 -1 0 -1.4703 0.0489
9 -1 1 -3.4717 -0.1371
9 -1 2 -0.2842 0.0451
9 -1 3 0.6832 0.0668
9 -1 4 -3.3444 -0.0866
9 -1 5 -0.3252 0.0376
9 -1 6 2.0679 0.0393
9 -1 7 1.7655 -0.0519
9 0 0 -0.1335 -0.0183
9 0 1 3.2943 0.0883
9 0 2 -3.1305 -0.0492
9 0 3 -6.4317 -0.0270
9 0 4 -1.2190 0.0504
9 0 5 2.1352 -0.0153
9 0 6 -4.9970 -0.0038
9 1 0 0.1313 -0.0200
9 1 1 -1.1162 -0.0547
9 1 2 -1.4904 0.0610
9 1 3 -2.7268 0.0089
9 1 4 0.3390 -0.0197
9 1 5 0.3679 0.0506
9 1 6 -0.9365 -0.0283
9 2 0 -4.3380 0.0442
9 2 1 -1.3607 0.0213
9 2 2 0.2038 -0.0126
9 2 3 -1.2300 -0.0107
9 2 4 -0.8812 0.0559
9 2 5 -0.1161 -0.0375
9 3 0 0.6359 -0.0846
9 3 1 -5.5764 -0.0085
9 3 2 -5.3853 0.0286
9 3 3 0.0689 -0.0329
9 4 0 -1.7963 0.0148
9 4 1 -5.5064 -0.0096
9 4 2 -5.3836 -0.0467
10 -11 0 2.6320 -0.0308
10 -11 1 -1.9403 0.0198
10 -11 2 -2.9631 0.0366
10 -10 0 -0.0709 0.0606
10 -10 1 1.6466 -0.0396
10 -10 2 1.0186 -0.0340
10 -10 3 -0.4049 0.0688
10 -9 0 -4.5205 -0.0484
10 -9 1 4.0845 -0.0276
10 -9 2 3.1522 0.0754
10 -9 3 -0.4117 -0.0292
10 -9 4 -3.5398 0.0043
10 -8 0 -1.3977 0.0030
10 -8 1 6.0687 0.0606
10 -8 2 4.0712 -0.0846
10 -8 3 -0.3647 0.0275
10 -8 4 3.2799 0.0430
10 -8 5 1.8055 -0.0345
10 -7 0 2.1072 0.0039
10 -7 1 0.6268 -0.0173
10 -7 2 0.6751 0.0444
10 -7 3 2.9045 0.0068
10 -7 4 -0.2886 -0.0546
10 -7 5 -5.5409 0.0351
10 -7 6 -3.7991 -0.0090
10 -6 0 -0.6947 0.0131
10 -6 1 -0.4193 -0.0221
10 -6 2 3.1751 -0.0035
10 -6 3 4.6008 0.0017
10 -6 4 -0.8795 0.0743
10 -6 5 -4.9789 -0.0578
10 -6 6 -6.2842 0.0018
10 -5 0 2.1805 -0.0687
10 -5 1 2.2643 0.0636
10 -5 2 3.9707 0.0052
10 -5 3 4.9199 -0.0208
10 -5 4 0.3292 -0.0206
10 -5 5 -6.8971 0.0523
10 -5 6 -3.6489 0.0041
10 -4 0 -1.0240 0.1220
10 -4 1 0.8727 -0.0757
10 -4 2 3.9837 -0.0016
10 -4 3 1.3090 0.0488
10 -4 4 -0.4735 -0.0108
10 -4 5 0.4262 -0.0286
10 -4 6 -2.2071 -0.0037
10 -3 0 -3.0065 -0.1444
10 -3 1 2.8802 0.0742
10 -3 2 1.3393 0.0502
10 -3 3 -3.0018 -0.0730
10 -3 4 3.6301 0.0323
10 -3 5 3.1485 0.0349
10 -3 6 -2.0768 -0.0130
10 -2 0 -0.4288 0.1316
10 -2 1 -0.7679 -0.0917
10 -2 2 0.6246 -0.0750
10 -2 3 2.5445 0.1007
10 -2 4 2.5614 -0.0090
10 -2 5 -0.5142 -0.0364
10 -1 0 -4.1373 -0.0694
10 -1 1 1.1912 0.0789
10 -1 2 1.9102 0.0167
10 -1 3 -0.9411 -0.1118
10 -1 4 -1.0608 0.0033
10 -1 5 3.5778 0.0150
10 0 0 -1.1164 0.0540
10 0 1 0.7117 -0.0565
10 0 2 -2.0439 -0.0466
10 0 3 -2.2645 0.0839
10 0 4 -0.8436 -0.0297
10 1 0 -2.3716 -0.0380
10 1 1 -2.3071 0.0285
10 1 2 0.9037 0.0178
10 1 3 -1.3197 -0.0268
10 2 0 1.4851 0.0504
10 2 1 -0.8126 -0.0621
10 2 2 -2.7192 0.0477
10 3 0 8.5489 -0.0040
11 -10 0 -0.0927 0.0371
11 -9 0 -6.2970 0.0496
11 -9 1 -1.2950 -0.0114
11 -9 2 1.3685 -0.0091
11 -8 0 -1.9238 -0.0578
11 -8 1 1.7103 0.0333
11 -8 2 1.9078 -0.0124
11 -8 3 -1.5157 0.0473
11 -7 0 -1.5117 0.0661
11 -7 1 0.5891 0.0259
11 -7 2 -1.0769 -0.0400
11 -7 3 0.2828 -0.0211
11 -6 0 -0.9931 -0.0374
11 -6 1 0.4325 -0.0604
11 -6 2 0.5752 0.0690
11 -6 3 4.3950 0.0002
11 -5 0 -1.6013 0.0505
11 -5 1 -0.8647 0.0387
11 -5 2 2.9081 -0.0666
11 -5 3 5.0776 0.0295
11 -4 0 -6.9067 -0.0738
11 -4 1 -2.5157 -0.0350
11 -4 2 3.7792 0.0919
11 -4 3 3.4444 -0.0700
11 -3 0 -5.4418 0.0862
11 -3 1 -3.3872 0.0302
11 -3 2 3.7834 -0.1528
11 -3 3 1.5369 0.0500
11 -2 0 -3.9387 -0.1104
11 -2 1 -1.6406 -0.0512
11 -2 2 3.4348 0.1267
11 -1 0 -0.7985 0.0602
11 -1 1 1.2501 0.0181
11 -1 2 0.3964 -0.0654
11 0 0 -1.0476 -0.1383
11 0 1 -0.3367 0.0195
12 -7 0 0.9453 0.0621
12 -6 0 4.9424 -0.0386
12 -5 0 2.3284 0.0162
12 -4 0 -0.0725 -0.0116
0 0 0 0.0 0.0
;
_iucr_refine_instructions_details
;
exp_17169.res created by SHELXL-2014/7
TITL exp_17169_a.res in P-1
REM Old TITL exp_17169_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.127, Rweak 0.019, Alpha 0.110, Orientation as input
REM Formula found by SHELXT: C20 Mo3 N9 O14
CELL 0.71073 10.6194 11.9177 14.7094 90.197 106.313 110.829
ZERR 1 0.0005 0.0005 0.001 0.004 0.005 0.004
LATT 1
SFAC C H Mo N O
UNIT 36 50 6 20 16
DFIX 0.88 0.01 N10 H10a
DFIX 0.85 0.01 O6 H6a
DFIX 1.5 0.01 C2 C1
DELU 0.01 0.005 C1 C3A
DELU 0.005 0.0025 O6 C1 Mo3 N7
DELU 0.00125 0.000625 Mo3 O3
DELU C18 C17 C17 N10 N10 C16 C15 C14 C14 N8 N8 C13 C2 O7 C2 O8 C1 C2
SIMU C18 C17 C17 N10 N10 C16 C15 C14 C14 N8 N8 C13 C2 O7 C2 O8 C1 C2
SIMU 0.01 0.02 3.8 $C
SIMU 0.005 0.01 3.8 $N
SIMU 0.0025 0.005 3.8 $O
ISOR 0.02 0.01 C3 C3A C2
ISOR 0.005 0.01 N8 N10
L.S. 20 0 0
PLAN 1
SIZE 0.2 0.1 0.04
TEMP -100.15
BOND $H
list 4
ABIN
fmap 2 53
acta
OMIT 0 50
REM
REM
REM
WGHT 0.049300 0.351100
FVAR 0.37507 0.49552
MO1 3 0.374816 0.587779 0.558563 11.00000 0.01986 0.01836 =
0.03293 0.00415 0.00686 0.00777
MO2 3 0.623584 0.618966 0.413973 11.00000 0.02052 0.01848 =
0.03084 0.00503 0.00780 0.00746
MO3 3 0.364645 0.508809 0.718644 11.00000 0.02675 0.02324 =
0.03221 0.00443 0.00889 0.01040
O2 5 0.752393 0.570728 0.508763 11.00000 0.02726 0.02280 =
0.03439 0.00662 0.01259 0.01135
O5 5 0.492869 0.626312 0.477202 11.00000 0.02861 0.02302 =
0.03315 0.00562 0.01128 0.01100
O1 5 0.523397 0.543208 0.656758 11.00000 0.02945 0.02655 =
0.03636 0.00662 0.01004 0.01279
O3 5 0.243801 0.346475 0.664976 11.00000 0.02966 0.02714 =
0.03766 0.00569 0.00873 0.01292
O4 5 0.259610 0.593517 0.643927 11.00000 0.02955 0.02724 =
0.03882 0.00542 0.01157 0.01251
O7 5 0.483573 0.299130 0.701377 11.00000 0.03295 0.03137 =
0.03907 0.00679 0.00920 0.01567
O8 5 0.483861 0.423298 0.818698 11.00000 0.03512 0.03272 =
0.04009 0.00782 0.00657 0.01389
N3 4 0.231083 0.655885 0.456977 11.00000 0.02673 0.01905 =
0.03501 0.00612 0.01264 0.01142
N5 4 0.752770 0.805046 0.483092 11.00000 0.03524 0.02075 =
0.03817 0.00375 0.01486 0.01042
N1 4 0.501071 0.779396 0.623002 11.00000 0.03347 0.02450 =
0.03888 0.00683 0.01329 0.01302
N4 4 0.037524 0.683031 0.381536 11.00000 0.02365 0.03017 =
0.04597 0.00547 0.00475 0.01445
AFIX 43
H4 2 -0.048035 0.684253 0.368673 11.00000 -1.20000
AFIX 0
N9 4 0.230603 0.485055 0.811462 11.00000 0.04714 0.04164 =
0.04387 0.00913 0.02109 0.01943
N6 4 0.916435 0.961075 0.576722 11.00000 0.03971 0.02317 =
0.04711 -0.00051 0.01210 0.00470
AFIX 43
H6 2 0.994994 1.006638 0.620102 11.00000 -1.20000
AFIX 0
N7 4 0.511197 0.664125 0.824626 11.00000 0.04403 0.03101 =
0.04110 0.00497 0.01096 0.01574
C7 1 0.102201 0.644592 0.457061 11.00000 0.02376 0.02932 =
0.03648 0.00872 0.00902 0.01026
AFIX 43
H7 2 0.061876 0.612591 0.505861 11.00000 -1.20000
AFIX 0
N2 4 0.678813 0.936313 0.703656 11.00000 0.04472 0.02976 =
0.04555 0.00257 0.01032 0.00735
AFIX 43
H2 2 0.764919 0.981936 0.738328 11.00000 -1.20000
AFIX 0
C10 1 0.878728 0.845180 0.550106 11.00000 0.03007 0.02478 =
0.04362 0.00622 0.01526 0.00708
AFIX 43
H10 2 0.932765 0.797367 0.574751 11.00000 -1.20000
AFIX 0
C4 1 0.635777 0.820124 0.672880 11.00000 0.03509 0.02463 =
0.04313 0.00165 0.01230 0.00997
AFIX 43
H4A 2 0.693544 0.773283 0.685021 11.00000 -1.20000
AFIX 0
C9 1 0.245638 0.703614 0.374405 11.00000 0.02826 0.03150 =
0.04417 0.00798 0.01654 0.01140
AFIX 43
H9 2 0.327423 0.721796 0.354119 11.00000 -1.20000
AFIX 0
C12 1 0.712735 0.903058 0.468379 11.00000 0.03567 0.03566 =
0.04864 0.01146 0.01157 0.01574
AFIX 43
H12 2 0.627745 0.903190 0.424712 11.00000 -1.20000
AFIX 0
O6 5 0.609177 0.183668 0.826546 11.00000 0.07468 0.05671 =
0.06451 0.00309 -0.00393 0.02524
C11 1 0.814429 0.997662 0.526294 11.00000 0.04187 0.02393 =
0.04608 0.00561 0.00819 0.01053
AFIX 43
H11 2 0.814700 1.077267 0.531075 11.00000 -1.20000
AFIX 0
C2 1 0.527670 0.341967 0.792629 11.00000 0.07289 0.01941 =
0.03604 0.00411 0.03734 0.01488
C8 1 0.126084 0.721319 0.325473 11.00000 0.02820 0.03661 =
0.04899 0.00920 0.01220 0.01382
AFIX 43
H8 2 0.107704 0.752934 0.266062 11.00000 -1.20000
AFIX 0
C6 1 0.460427 0.875754 0.623582 11.00000 0.04125 0.03002 =
0.05986 -0.00247 0.00838 0.01743
AFIX 43
H6B 2 0.368112 0.874243 0.593171 11.00000 -1.20000
AFIX 0
C16 1 0.141065 0.538564 0.812216 11.00000 0.07826 0.05901 =
0.05100 0.01686 0.03613 0.03209
AFIX 43
H16 2 0.123805 0.595521 0.770293 11.00000 -1.20000
AFIX 0
C15 1 0.649259 0.688049 0.873368 11.00000 0.04351 0.03987 =
0.05243 0.00109 -0.00374 0.01272
AFIX 43
H15 2 0.699969 0.637670 0.869195 11.00000 -1.20000
AFIX 0
C18 1 0.219075 0.411427 0.879305 11.00000 0.08804 0.08167 =
0.04183 0.02244 0.03792 0.04884
AFIX 43
H18 2 0.270220 0.359479 0.895511 11.00000 -1.20000
AFIX 0
C5 1 0.570389 0.972831 0.673526 11.00000 0.04581 0.03110 =
0.06170 -0.00601 0.00743 0.01776
AFIX 43
H5 2 0.571104 1.051551 0.685139 11.00000 -1.20000
AFIX 0
C13 1 0.482649 0.758204 0.850742 11.00000 0.05434 0.04126 =
0.05589 -0.00390 0.00306 0.01502
AFIX 43
H13 2 0.393532 0.766315 0.828990 11.00000 -1.20000
AFIX 0
C17 1 0.127002 0.420161 0.921162 11.00000 0.08944 0.09058 =
0.05471 0.03014 0.04856 0.05242
AFIX 43
H17 2 0.100703 0.376625 0.971138 11.00000 -1.20000
AFIX 0
N8 4 0.601073 0.840166 0.913185 11.00000 0.06452 0.04590 =
0.05653 -0.00300 0.00679 0.01499
AFIX 43
H8A 2 0.609343 0.910262 0.938778 11.00000 -1.20000
AFIX 0
N10 4 0.078252 0.502420 0.879201 11.00000 0.07024 0.07267 =
0.06709 0.01028 0.02909 0.02939
AFIX 43
H10A 2 0.016715 0.527602 0.893220 11.00000 -1.20000
AFIX 0
C1 1 0.605280 0.289961 0.864198 11.00000 0.07603 0.05672 =
0.05017 -0.00573 0.01332 0.02949
PART 1
AFIX 13
H1A 2 0.705099 0.348439 0.879289 21.00000 -1.20000
AFIX 13
PART 0
PART 2
H1B 2 0.566184 0.275490 0.919368 -21.00000 -1.20000
AFIX 0
PART 0
C14 1 0.702368 0.794736 0.928488 11.00000 0.05056 0.04495 =
0.05504 -0.00305 -0.01517 0.00402
AFIX 43
H14 2 0.795598 0.831175 0.970813 11.00000 -1.20000
AFIX 0
PART 1
C3 1 0.581459 0.283554 0.947235 21.00000 0.07316 0.07040 =
0.06741 0.00965 0.02217 0.04297
AFIX 137
H3A 2 0.492064 0.216780 0.941771 21.00000 -1.50000
H3B 2 0.575850 0.359585 0.967550 21.00000 -1.50000
H3C 2 0.658674 0.269513 0.994394 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C3A 1 0.741876 0.378023 0.891284 -21.00000 0.07736 0.07581 =
0.08222 0.01077 0.01085 0.02728
AFIX 137
H3AA 2 0.804233 0.350679 0.940867 -21.00000 -1.50000
H3AB 2 0.740069 0.453651 0.916142 -21.00000 -1.50000
H3AC 2 0.777088 0.391474 0.835834 -21.00000 -1.50000
AFIX 3
PART 0
H6A 2 0.603876 0.113973 0.851785 11.00000 -1.20000
AFIX 0
HKLF 4
REM exp_17169_a.res in P-1
REM R1 = 0.0520 for 4536 Fo > 4sig(Fo) and 0.0689 for all 5853 data
REM 364 parameters refined using 419 restraints
END
WGHT 0.0493 0.3511
REM Highest difference peak 1.153, deepest hole -1.031, 1-sigma level 0.121
Q1 1 0.5998 0.3543 0.8273 11.00000 0.05 1.15
REM The information below was added by Olex2.
REM
REM R1 = 0.0520 for 4536 Fo > 4sig(Fo) and 0.0689 for all 14515 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.15, deepest hole -1.03
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0689
REM R1_gt = 0.0520
REM wR_ref = 0.1199
REM GOOF = 1.031
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 14515
REM Reflections_gt = 4536
REM Parameters = n/a
REM Hole = -1.03
REM Peak = 1.15
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.930