# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017
#######################################################################
#
# 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_hk-5-182
_database_code_depnum_ccdc_archive 'CCDC 1553741'
_audit_update_record
;
2017-06-02 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_audit_creation_date 2017-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C5 H9 Mo3 O20 V3, 2(C16 H36 N), C2 H3 N'
_chemical_formula_sum 'C39 H84 Mo3 N3 O20 V3'
_chemical_formula_weight 1355.73
_chemical_melting_point ?
_chemical_oxdiff_formula V3Mo3O22C18N2
_chemical_oxdiff_usercomment 'V3Mo3O19(CH2)3CH2OH '
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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 monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 15.7895(2)
_cell_length_b 18.8620(3)
_cell_length_c 18.1257(2)
_cell_angle_alpha 90
_cell_angle_beta 98.4590(10)
_cell_angle_gamma 90
_cell_volume 5339.50(12)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 8478
_cell_measurement_temperature 130.00(10)
_cell_measurement_theta_max 74.5410
_cell_measurement_theta_min 4.1570
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 10.447
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.67885
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43i (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.686
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description rod
_exptl_crystal_F_000 2776
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.07
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0224
_diffrn_reflns_av_unetI/netI 0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 22122
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.732
_diffrn_reflns_theta_min 3.401
_diffrn_ambient_environment air
_diffrn_ambient_temperature 130.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_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 -49.00 31.00 1.00 2.50 -- -40.81 38.00 -90.00 80
2 \w 56.00 98.00 1.00 2.50 -- 40.81-125.00 -90.00 42
3 \w 43.00 95.00 1.00 7.50 -- 107.94 -45.00-150.00 52
4 \w 62.00 89.00 1.00 7.50 -- 107.94 -30.00 -90.00 27
5 \w 83.00 173.00 1.00 7.50 -- 107.94 30.00-180.00 90
6 \w 43.00 85.00 1.00 7.50 -- 107.94 -45.00 30.00 42
7 \w 37.00 109.00 1.00 7.50 -- 107.94 -94.00 60.00 72
8 \w 80.00 108.00 1.00 7.50 -- 107.94 -94.00 150.00 28
9 \w 24.00 52.00 1.00 7.50 -- 107.94 -94.00 150.00 28
10 \w 33.00 88.00 1.00 7.50 -- 107.94 -30.00 -30.00 55
11 \w 36.00 76.00 1.00 7.50 -- 107.94 -45.00 -90.00 40
12 \w 152.00 177.00 1.00 7.50 -- 107.94 111.00 90.00 25
13 \w -96.00 -70.00 1.00 2.50 -- -40.81 125.00 90.00 26
14 \w -113.00 -14.00 1.00 2.50 -- -40.81 -57.00 120.00 99
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0610135000
_diffrn_orient_matrix_UB_12 -0.0261547000
_diffrn_orient_matrix_UB_13 0.0687784000
_diffrn_orient_matrix_UB_21 -0.0540456000
_diffrn_orient_matrix_UB_22 0.0391720000
_diffrn_orient_matrix_UB_23 0.0513949000
_diffrn_orient_matrix_UB_31 -0.0555302000
_diffrn_orient_matrix_UB_32 -0.0667416000
_diffrn_orient_matrix_UB_33 0.0031986000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 9257
_reflns_number_total 10668
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 67.62
_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 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43i (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 0.853
_refine_diff_density_min -0.967
_refine_diff_density_rms 0.077
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 634
_refine_ls_number_reflns 10668
_refine_ls_number_restraints 4
_refine_ls_R_factor_all 0.0370
_refine_ls_R_factor_gt 0.0306
_refine_ls_restrained_S_all 1.100
_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^)+(0.0418P)^2^+3.3214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0804
_refine_ls_wR_factor_ref 0.0854
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups, All C(H,H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2. Shared sites
{V1, Mo1}
{Mo2, V2}
{Mo3, V3}
{V6, Mo6}
{V5, Mo5}
{V4, Mo4}
3. Restrained distances
C19-C21
1.5 with sigma of 0.02
C21-C20
1.5 with sigma of 0.02
C21'-C20'
1.5 with sigma of 0.02
C20'-C19'
1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Mo1) = Uanis(V1)
Uanis(V2) = Uanis(Mo2)
Uanis(V3) = Uanis(Mo3)
Uanis(Mo4) = Uanis(V4)
Uanis(Mo5) = Uanis(V5)
Uanis(Mo6) = Uanis(V6)
Uanis(C19') = Uanis(C19)
Uanis(C21) = Uanis(C21')
Uanis(C20) = Uanis(C20')
Uanis(V1) = Uanis(Mo1)
Uanis(Mo2) = Uanis(V2)
Uanis(Mo3) = Uanis(V3)
Uanis(V6) = Uanis(Mo6)
Uanis(V5) = Uanis(Mo5)
Uanis(V4) = Uanis(Mo4)
5. Others
Sof(H18C)=Sof(H18D)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=
Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(1)
Sof(H18A)=Sof(H18B)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20C)=
Sof(H20D)=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=FVAR(1)
Fixed Sof: Mo1(0.5) Mo2(0.25) Mo3(0.25) Mo4(0.75) Mo5(0.5) Mo6(0.75) V1(0.5)
V2(0.75) V3(0.75) V4(0.25) V5(0.5) V6(0.25)
6.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C18(H18C,H18D), C19(H19A,H19B),
C19'(H19C,H19D), C20(H20A,H20B), C20'(H20C,H20D), C22(H22A,H22B), C23(H23A,
H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,H35B),
C36(H36A,H36B)
6.b Idealised Me refined as rotating group:
C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,
H21C), C21'(H21D,H21E,H21F), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C),
C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C)
6.c Idealised tetrahedral OH refined as rotating group:
O20(H20)
;
_atom_sites_solution_hydrogens geom
_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 0.81103(2) 0.56470(2) 0.64259(2) 0.02322(7) Uani 0.5 1 d . . P A 16
Mo2 Mo 0.75151(2) 0.43940(2) 0.75775(2) 0.02051(8) Uani 0.25 1 d . . P A 17
Mo3 Mo 0.60882(2) 0.55970(2) 0.67908(2) 0.02081(8) Uani 0.25 1 d . . P A 19
Mo4 Mo 0.67817(2) 0.56146(2) 0.85115(2) 0.02796(7) Uani 0.75 1 d . . P A 26
Mo5 Mo 0.73835(2) 0.67989(2) 0.74138(2) 0.02499(7) Uani 0.5 1 d . . P A 24
Mo6 Mo 0.87520(2) 0.56474(2) 0.81768(2) 0.02552(7) Uani 0.75 1 d . . P A 22
V1 V 0.81103(2) 0.56470(2) 0.64259(2) 0.02322(7) Uani 0.5 1 d . . P A 15
V2 V 0.75151(2) 0.43940(2) 0.75775(2) 0.02051(8) Uani 0.75 1 d . . P A 18
V3 V 0.60882(2) 0.55970(2) 0.67908(2) 0.02081(8) Uani 0.75 1 d . . P A 20
V4 V 0.67817(2) 0.56146(2) 0.85115(2) 0.02796(7) Uani 0.25 1 d . . P A 25
V5 V 0.73835(2) 0.67989(2) 0.74138(2) 0.02499(7) Uani 0.5 1 d . . P A 23
V6 V 0.87520(2) 0.56474(2) 0.81768(2) 0.02552(7) Uani 0.25 1 d . . P A 21
O1 O 0.84862(12) 0.55588(10) 0.56278(11) 0.0297(4) Uani 1 1 d . . . . .
O2 O 0.68356(10) 0.55132(9) 0.59652(9) 0.0222(3) Uani 1 1 d . . . . .
O3 O 0.78722(11) 0.65744(9) 0.65164(10) 0.0269(4) Uani 1 1 d . . . . .
O4 O 0.79725(10) 0.45604(9) 0.65834(9) 0.0199(3) Uani 1 1 d . . . . .
O5 O 0.90341(10) 0.56166(9) 0.71439(10) 0.0238(3) Uani 1 1 d . . . . .
O6 O 0.74226(9) 0.55618(8) 0.74111(8) 0.0187(3) Uani 1 1 d . . . . .
O7 O 0.75386(11) 0.35406(11) 0.75314(10) 0.0312(4) Uani 1 1 d . . . . .
O8 O 0.85849(11) 0.46400(9) 0.80373(10) 0.0258(4) Uani 1 1 d . . . . .
O9 O 0.69696(11) 0.45996(10) 0.83619(10) 0.0270(4) Uani 1 1 d . . . . .
O10 O 0.63662(10) 0.45316(9) 0.68954(9) 0.0207(3) Uani 1 1 d . . . . .
O11 O 0.51858(11) 0.55188(10) 0.62430(11) 0.0298(4) Uani 1 1 d . . . . .
O12 O 0.63026(11) 0.65321(9) 0.68284(10) 0.0272(4) Uani 1 1 d . . . . .
O13 O 0.58263(11) 0.55365(9) 0.77465(10) 0.0261(4) Uani 1 1 d . . . . .
O14 O 0.63405(14) 0.56180(11) 0.92925(12) 0.0391(5) Uani 1 1 d . . . . .
O15 O 0.68726(11) 0.65766(10) 0.82706(10) 0.0286(4) Uani 1 1 d . . . . .
O16 O 0.79964(12) 0.56319(10) 0.88769(10) 0.0288(4) Uani 1 1 d . . . . .
O17 O 0.73278(12) 0.76715(10) 0.73772(13) 0.0379(5) Uani 1 1 d . . . . .
O18 O 0.84684(11) 0.66206(9) 0.79630(10) 0.0258(4) Uani 1 1 d . . . . .
O19 O 0.97112(13) 0.56998(11) 0.86957(12) 0.0368(4) Uani 1 1 d . . . . .
O20 O 0.65339(13) 0.30230(11) 0.51803(13) 0.0405(5) Uani 1 1 d . . . . .
H20 H 0.7012 0.2881 0.5129 0.061 Uiso 1 1 calc GR . . . .
C1 C 0.66054(15) 0.50090(14) 0.53776(13) 0.0250(5) Uani 1 1 d . . . . .
H1A H 0.6954 0.5089 0.4987 0.030 Uiso 1 1 calc R . . . .
H1B H 0.6011 0.5080 0.5165 0.030 Uiso 1 1 calc R . . . .
C2 C 0.61625(15) 0.40893(13) 0.62483(13) 0.0236(5) Uani 1 1 d . . . . .
H2A H 0.5568 0.4161 0.6038 0.028 Uiso 1 1 calc R . . . .
H2B H 0.6232 0.3596 0.6397 0.028 Uiso 1 1 calc R . . . .
C3 C 0.76618(15) 0.41095(13) 0.59660(13) 0.0238(5) Uani 1 1 d . . . . .
H3A H 0.7726 0.3619 0.6125 0.029 Uiso 1 1 calc R . . . .
H3B H 0.8009 0.4181 0.5573 0.029 Uiso 1 1 calc R . . . .
C4 C 0.67274(15) 0.42456(13) 0.56538(14) 0.0235(5) Uani 1 1 d . . . . .
C5 C 0.64587(17) 0.37526(15) 0.49856(15) 0.0317(6) Uani 1 1 d . . . . .
H5A H 0.5869 0.3853 0.4777 0.038 Uiso 1 1 calc R . . . .
H5B H 0.6813 0.3851 0.4603 0.038 Uiso 1 1 calc R . . . .
N1 N 0.49808(14) 0.83164(12) 0.62059(13) 0.0300(5) Uani 1 1 d . . . . .
C6 C 0.41852(16) 0.84483(14) 0.56439(16) 0.0294(5) Uani 1 1 d . . . . .
H6A H 0.4023 0.8006 0.5388 0.035 Uiso 1 1 calc R . . . .
H6B H 0.3723 0.8581 0.5914 0.035 Uiso 1 1 calc R . . . .
C7 C 0.42625(17) 0.90119(14) 0.50622(16) 0.0312(5) Uani 1 1 d . . . . .
H7A H 0.4708 0.8881 0.4772 0.037 Uiso 1 1 calc R . . . .
H7B H 0.4418 0.9461 0.5305 0.037 Uiso 1 1 calc R . . . .
C8 C 0.34109(19) 0.90838(16) 0.45525(19) 0.0411(7) Uani 1 1 d . . . . .
H8A H 0.3269 0.8636 0.4302 0.049 Uiso 1 1 calc R . . . .
H8B H 0.2965 0.9192 0.4851 0.049 Uiso 1 1 calc R . . . .
C9 C 0.3435(2) 0.96596(18) 0.3974(2) 0.0525(9) Uani 1 1 d . . . . .
H9A H 0.3542 1.0109 0.4219 0.079 Uiso 1 1 calc GR . . . .
H9B H 0.2896 0.9676 0.3652 0.079 Uiso 1 1 calc GR . . . .
H9C H 0.3884 0.9559 0.3684 0.079 Uiso 1 1 calc GR . . . .
C10 C 0.57661(16) 0.81911(15) 0.58227(15) 0.0301(5) Uani 1 1 d . . . . .
H10A H 0.5888 0.8625 0.5571 0.036 Uiso 1 1 calc R . . . .
H10B H 0.6252 0.8096 0.6203 0.036 Uiso 1 1 calc R . . . .
C11 C 0.56914(18) 0.75914(15) 0.52618(16) 0.0332(6) Uani 1 1 d . . . . .
H11A H 0.5222 0.7684 0.4865 0.040 Uiso 1 1 calc R . . . .
H11B H 0.5574 0.7151 0.5503 0.040 Uiso 1 1 calc R . . . .
C12 C 0.6524(2) 0.75272(17) 0.49396(17) 0.0401(7) Uani 1 1 d . . . . .
H12A H 0.6632 0.7969 0.4696 0.048 Uiso 1 1 calc R . . . .
H12B H 0.6991 0.7451 0.5343 0.048 Uiso 1 1 calc R . . . .
C13 C 0.6510(2) 0.69285(18) 0.4386(2) 0.0521(9) Uani 1 1 d . . . . .
H13A H 0.6403 0.6490 0.4624 0.078 Uiso 1 1 calc GR . . . .
H13B H 0.7053 0.6903 0.4209 0.078 Uiso 1 1 calc GR . . . .
H13C H 0.6066 0.7011 0.3974 0.078 Uiso 1 1 calc GR . . . .
C14 C 0.51319(18) 0.89688(16) 0.67028(16) 0.0359(6) Uani 1 1 d . . . . .
H14A H 0.5142 0.9382 0.6386 0.043 Uiso 1 1 calc R . . . .
H14B H 0.4649 0.9021 0.6973 0.043 Uiso 1 1 calc R . . . .
C15 C 0.59432(19) 0.89643(19) 0.72601(17) 0.0429(7) Uani 1 1 d . . . . .
H15A H 0.5990 0.8519 0.7531 0.051 Uiso 1 1 calc R . . . .
H15B H 0.6436 0.9008 0.7001 0.051 Uiso 1 1 calc R . . . .
C16 C 0.59310(19) 0.95715(19) 0.77993(17) 0.0427(7) Uani 1 1 d . . . . .
H16A H 0.5719 0.9992 0.7523 0.051 Uiso 1 1 calc R . . . .
H16B H 0.5535 0.9459 0.8144 0.051 Uiso 1 1 calc R . . . .
C17 C 0.6794(2) 0.9735(2) 0.82391(18) 0.0515(9) Uani 1 1 d . . . . .
H17A H 0.7020 0.9317 0.8499 0.077 Uiso 1 1 calc GR . . . .
H17B H 0.6736 1.0104 0.8593 0.077 Uiso 1 1 calc GR . . . .
H17C H 0.7177 0.9888 0.7906 0.077 Uiso 1 1 calc GR . . . .
C18 C 0.4839(2) 0.76589(17) 0.66571(18) 0.0437(8) Uani 1 1 d . . . . .
H18A H 0.5298 0.7630 0.7075 0.052 Uiso 0.531(4) 1 calc R . P B 1
H18B H 0.4883 0.7246 0.6346 0.052 Uiso 0.531(4) 1 calc R . P B 1
H18C H 0.5391 0.7459 0.6857 0.052 Uiso 0.469(4) 1 calc R . P B 2
H18D H 0.4533 0.7309 0.6327 0.052 Uiso 0.469(4) 1 calc R . P B 2
C19 C 0.4329(4) 0.7803(4) 0.7309(4) 0.0383(10) Uani 0.469(4) 1 d D . P B 2
H19A H 0.4626 0.8158 0.7638 0.046 Uiso 0.469(4) 1 calc R . P B 2
H19B H 0.3768 0.7988 0.7113 0.046 Uiso 0.469(4) 1 calc R . P B 2
C19' C 0.3955(4) 0.7616(3) 0.6973(3) 0.0383(10) Uani 0.531(4) 1 d D . P B 1
H19C H 0.3867 0.8047 0.7245 0.046 Uiso 0.531(4) 1 calc R . P B 1
H19D H 0.3487 0.7569 0.6565 0.046 Uiso 0.531(4) 1 calc R . P B 1
C20 C 0.4232(6) 0.7145(5) 0.7737(4) 0.0406(12) Uani 0.469(4) 1 d D . P B 2
H20A H 0.4783 0.6923 0.7893 0.049 Uiso 0.469(4) 1 calc R . P B 2
H20B H 0.3965 0.7245 0.8174 0.049 Uiso 0.469(4) 1 calc R . P B 2
C20' C 0.3971(5) 0.6969(4) 0.7498(4) 0.0406(12) Uani 0.531(4) 1 d D . P B 1
H20C H 0.3406 0.6921 0.7641 0.049 Uiso 0.531(4) 1 calc R . P B 1
H20D H 0.4070 0.6550 0.7212 0.049 Uiso 0.531(4) 1 calc R . P B 1
C21 C 0.3704(6) 0.6710(4) 0.7233(4) 0.0514(13) Uani 0.469(4) 1 d D . P B 2
H21A H 0.3217 0.6977 0.7006 0.077 Uiso 0.469(4) 1 calc GR . P B 2
H21B H 0.3515 0.6312 0.7495 0.077 Uiso 0.469(4) 1 calc GR . P B 2
H21C H 0.4021 0.6545 0.6854 0.077 Uiso 0.469(4) 1 calc GR . P B 2
C21' C 0.4599(4) 0.6964(4) 0.8184(3) 0.0514(13) Uani 0.531(4) 1 d D . P B 1
H21D H 0.5160 0.7055 0.8062 0.077 Uiso 0.531(4) 1 calc GR . P B 1
H21E H 0.4594 0.6508 0.8420 0.077 Uiso 0.531(4) 1 calc GR . P B 1
H21F H 0.4454 0.7324 0.8518 0.077 Uiso 0.531(4) 1 calc GR . P B 1
N2 N 0.96201(12) 0.85347(11) 0.83345(11) 0.0206(4) Uani 1 1 d . . . . .
C22 C 0.90058(15) 0.85398(13) 0.76106(13) 0.0232(5) Uani 1 1 d . . . . .
H22A H 0.8453 0.8700 0.7718 0.028 Uiso 1 1 calc R . . . .
H22B H 0.8935 0.8055 0.7433 0.028 Uiso 1 1 calc R . . . .
C23 C 0.92473(17) 0.89912(14) 0.69811(14) 0.0288(5) Uani 1 1 d . . . . .
H23A H 0.9745 0.8793 0.6800 0.035 Uiso 1 1 calc R . . . .
H23B H 0.9385 0.9469 0.7157 0.035 Uiso 1 1 calc R . . . .
C24 C 0.84838(19) 0.90042(16) 0.63536(15) 0.0360(6) Uani 1 1 d . . . . .
H24A H 0.8336 0.8521 0.6202 0.043 Uiso 1 1 calc R . . . .
H24B H 0.7995 0.9210 0.6542 0.043 Uiso 1 1 calc R . . . .
C25 C 0.8660(3) 0.94217(19) 0.56815(17) 0.0510(8) Uani 1 1 d . . . . .
H25A H 0.8152 0.9436 0.5319 0.076 Uiso 1 1 calc GR . . . .
H25B H 0.9113 0.9199 0.5468 0.076 Uiso 1 1 calc GR . . . .
H25C H 0.8826 0.9896 0.5831 0.076 Uiso 1 1 calc GR . . . .
C26 C 0.98401(15) 0.92855(12) 0.85972(13) 0.0207(4) Uani 1 1 d . . . . .
H26A H 1.0216 0.9263 0.9071 0.025 Uiso 1 1 calc R . . . .
H26B H 1.0155 0.9512 0.8241 0.025 Uiso 1 1 calc R . . . .
C27 C 0.90758(15) 0.97434(13) 0.86914(14) 0.0249(5) Uani 1 1 d . . . . .
H27A H 0.8739 0.9511 0.9027 0.030 Uiso 1 1 calc R . . . .
H27B H 0.8717 0.9801 0.8212 0.030 Uiso 1 1 calc R . . . .
C28 C 0.93577(16) 1.04677(14) 0.90026(15) 0.0289(5) Uani 1 1 d . . . . .
H28A H 0.9719 1.0691 0.8680 0.035 Uiso 1 1 calc R . . . .
H28B H 0.9692 1.0412 0.9493 0.035 Uiso 1 1 calc R . . . .
C29 C 0.85853(17) 1.09422(15) 0.90609(16) 0.0333(6) Uani 1 1 d . . . . .
H29A H 0.8276 1.1025 0.8572 0.050 Uiso 1 1 calc GR . . . .
H29B H 0.8778 1.1386 0.9284 0.050 Uiso 1 1 calc GR . . . .
H29C H 0.8217 1.0713 0.9364 0.050 Uiso 1 1 calc GR . . . .
C30 C 0.91670(14) 0.81323(13) 0.88945(13) 0.0226(5) Uani 1 1 d . . . . .
H30A H 0.8615 0.8353 0.8909 0.027 Uiso 1 1 calc R . . . .
H30B H 0.9062 0.7651 0.8715 0.027 Uiso 1 1 calc R . . . .
C31 C 0.96427(16) 0.81016(14) 0.96774(13) 0.0259(5) Uani 1 1 d . . . . .
H31A H 0.9727 0.8579 0.9873 0.031 Uiso 1 1 calc R . . . .
H31B H 1.0202 0.7891 0.9670 0.031 Uiso 1 1 calc R . . . .
C32 C 0.9157(2) 0.76697(16) 1.01855(16) 0.0394(7) Uani 1 1 d . . . . .
H32A H 0.8588 0.7867 1.0175 0.047 Uiso 1 1 calc R . . . .
H32B H 0.9096 0.7186 1.0003 0.047 Uiso 1 1 calc R . . . .
C33 C 0.9615(2) 0.76662(16) 1.09823(16) 0.0403(7) Uani 1 1 d . . . . .
H33A H 1.0167 0.7450 1.0998 0.060 Uiso 1 1 calc GR . . . .
H33B H 0.9283 0.7402 1.1291 0.060 Uiso 1 1 calc GR . . . .
H33C H 0.9683 0.8144 1.1162 0.060 Uiso 1 1 calc GR . . . .
C34 C 1.04614(14) 0.81807(12) 0.82385(13) 0.0221(5) Uani 1 1 d . . . . .
H34A H 1.0872 0.8277 0.8680 0.026 Uiso 1 1 calc R . . . .
H34B H 1.0676 0.8402 0.7820 0.026 Uiso 1 1 calc R . . . .
C35 C 1.04317(15) 0.73816(13) 0.81099(14) 0.0251(5) Uani 1 1 d . . . . .
H35A H 0.9995 0.7269 0.7692 0.030 Uiso 1 1 calc R . . . .
H35B H 1.0287 0.7143 0.8549 0.030 Uiso 1 1 calc R . . . .
C36 C 1.13034(17) 0.71260(14) 0.79483(16) 0.0302(5) Uani 1 1 d . . . . .
H36A H 1.1397 0.7300 0.7463 0.036 Uiso 1 1 calc R . . . .
H36B H 1.1748 0.7321 0.8319 0.036 Uiso 1 1 calc R . . . .
C37 C 1.13685(19) 0.63215(15) 0.79578(17) 0.0364(6) Uani 1 1 d . . . . .
H37A H 1.0931 0.6127 0.7590 0.055 Uiso 1 1 calc GR . . . .
H37B H 1.1295 0.6148 0.8442 0.055 Uiso 1 1 calc GR . . . .
H37C H 1.1921 0.6182 0.7848 0.055 Uiso 1 1 calc GR . . . .
N3 N 0.81118(19) 0.23061(15) 0.49557(19) 0.0513(7) Uani 1 1 d . . . . .
C38 C 0.84294(19) 0.17890(16) 0.48137(17) 0.0371(6) Uani 1 1 d . . . . .
C39 C 0.8840(2) 0.11306(17) 0.46421(18) 0.0440(7) Uani 1 1 d . . . . .
H39A H 0.9056 0.1179 0.4177 0.066 Uiso 1 1 calc GR . . . .
H39B H 0.8430 0.0751 0.4605 0.066 Uiso 1 1 calc GR . . . .
H39C H 0.9305 0.1027 0.5031 0.066 Uiso 1 1 calc GR . . . .
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 0.01782(13) 0.03038(15) 0.02214(13) 0.00187(10) 0.00523(10) 0.00005(10)
Mo2 0.01685(15) 0.02279(17) 0.02186(15) 0.00093(11) 0.00276(12) -0.00127(11)
Mo3 0.01339(14) 0.02426(16) 0.02426(16) -0.00130(12) 0.00106(11) 0.00087(11)
Mo4 0.02774(13) 0.03527(14) 0.02285(12) -0.00445(9) 0.01026(9) -0.00392(9)
Mo5 0.01903(13) 0.01762(13) 0.03707(15) -0.00051(10) 0.00001(10) -0.00154(9)
Mo6 0.01680(11) 0.03200(13) 0.02592(12) 0.00074(9) -0.00297(8) -0.00290(8)
V1 0.01782(13) 0.03038(15) 0.02214(13) 0.00187(10) 0.00523(10) 0.00005(10)
V2 0.01685(15) 0.02279(17) 0.02186(15) 0.00093(11) 0.00276(12) -0.00127(11)
V3 0.01339(14) 0.02426(16) 0.02426(16) -0.00130(12) 0.00106(11) 0.00087(11)
V4 0.02774(13) 0.03527(14) 0.02285(12) -0.00445(9) 0.01026(9) -0.00392(9)
V5 0.01903(13) 0.01762(13) 0.03707(15) -0.00051(10) 0.00001(10) -0.00154(9)
V6 0.01680(11) 0.03200(13) 0.02592(12) 0.00074(9) -0.00297(8) -0.00290(8)
O1 0.0239(9) 0.0367(10) 0.0294(9) -0.0007(8) 0.0073(7) -0.0026(7)
O2 0.0181(8) 0.0270(8) 0.0211(8) 0.0005(7) 0.0019(6) 0.0005(6)
O3 0.0241(8) 0.0263(9) 0.0307(9) 0.0044(7) 0.0054(7) -0.0023(7)
O4 0.0170(7) 0.0231(8) 0.0200(7) -0.0008(6) 0.0036(6) -0.0007(6)
O5 0.0167(8) 0.0289(9) 0.0263(8) -0.0023(7) 0.0049(6) -0.0035(6)
O6 0.0150(7) 0.0238(8) 0.0176(7) -0.0011(6) 0.0038(6) -0.0013(6)
O7 0.0260(9) 0.0313(10) 0.0364(10) 0.0054(8) 0.0053(8) 0.0000(7)
O8 0.0197(8) 0.0305(9) 0.0254(8) 0.0038(7) -0.0023(7) -0.0001(7)
O9 0.0258(9) 0.0317(9) 0.0241(8) 0.0023(7) 0.0054(7) -0.0032(7)
O10 0.0156(7) 0.0256(8) 0.0213(8) -0.0026(6) 0.0036(6) -0.0011(6)
O11 0.0197(8) 0.0371(10) 0.0322(9) 0.0005(8) 0.0022(7) 0.0032(7)
O12 0.0209(8) 0.0255(8) 0.0356(9) -0.0002(7) 0.0051(7) 0.0051(7)
O13 0.0173(8) 0.0331(9) 0.0289(9) -0.0057(7) 0.0069(7) -0.0015(7)
O14 0.0403(11) 0.0469(12) 0.0330(10) -0.0044(9) 0.0149(9) -0.0090(9)
O15 0.0236(8) 0.0294(9) 0.0335(9) -0.0075(8) 0.0068(7) -0.0010(7)
O16 0.0246(9) 0.0382(10) 0.0227(9) -0.0025(7) 0.0002(7) -0.0051(7)
O17 0.0272(9) 0.0272(10) 0.0591(13) -0.0028(9) 0.0053(9) -0.0020(8)
O18 0.0212(8) 0.0278(9) 0.0283(9) -0.0050(7) 0.0033(7) -0.0043(7)
O19 0.0273(10) 0.0437(11) 0.0370(11) 0.0016(9) -0.0038(8) -0.0042(8)
O20 0.0339(10) 0.0359(10) 0.0522(12) -0.0161(10) 0.0075(9) -0.0033(8)
C1 0.0213(11) 0.0347(13) 0.0183(10) -0.0019(9) 0.0010(9) 0.0005(10)
C2 0.0180(10) 0.0282(12) 0.0240(11) -0.0056(9) 0.0011(9) -0.0020(9)
C3 0.0213(11) 0.0276(12) 0.0237(11) -0.0050(9) 0.0070(9) 0.0007(9)
C4 0.0190(11) 0.0284(12) 0.0228(11) -0.0036(9) 0.0019(9) -0.0009(9)
C5 0.0263(12) 0.0394(14) 0.0286(13) -0.0117(11) 0.0014(10) -0.0022(11)
N1 0.0246(10) 0.0355(12) 0.0310(11) 0.0010(9) 0.0079(9) 0.0098(9)
C6 0.0206(11) 0.0286(12) 0.0393(14) -0.0006(11) 0.0050(10) 0.0023(10)
C7 0.0261(12) 0.0309(13) 0.0356(14) 0.0006(11) 0.0009(11) -0.0016(10)
C8 0.0336(15) 0.0344(15) 0.0508(18) 0.0023(13) -0.0092(13) -0.0011(12)
C9 0.057(2) 0.0443(18) 0.0489(19) 0.0051(15) -0.0159(16) 0.0051(16)
C10 0.0212(12) 0.0390(14) 0.0312(13) -0.0017(11) 0.0073(10) 0.0065(10)
C11 0.0325(14) 0.0318(14) 0.0382(14) -0.0005(11) 0.0149(12) 0.0055(11)
C12 0.0384(16) 0.0473(17) 0.0380(15) -0.0004(13) 0.0172(13) 0.0056(13)
C13 0.060(2) 0.0445(18) 0.059(2) -0.0056(16) 0.0315(18) 0.0095(16)
C14 0.0280(13) 0.0440(16) 0.0351(14) -0.0082(12) 0.0027(11) 0.0120(12)
C15 0.0328(15) 0.061(2) 0.0336(15) -0.0060(14) 0.0026(12) 0.0171(14)
C16 0.0292(14) 0.064(2) 0.0336(15) -0.0082(14) 0.0021(12) 0.0066(14)
C17 0.0346(16) 0.083(3) 0.0351(16) -0.0012(16) -0.0006(13) 0.0045(16)
C18 0.0477(18) 0.0449(17) 0.0443(17) 0.0154(14) 0.0259(14) 0.0203(14)
C19 0.035(3) 0.047(3) 0.036(3) 0.004(2) 0.0153(19) 0.005(2)
C19' 0.035(3) 0.047(3) 0.036(3) 0.004(2) 0.0153(19) 0.005(2)
C20 0.046(4) 0.052(4) 0.024(4) -0.012(3) 0.008(3) -0.011(3)
C20' 0.046(4) 0.052(4) 0.024(4) -0.012(3) 0.008(3) -0.011(3)
C21 0.058(3) 0.064(3) 0.035(3) 0.015(2) 0.017(2) 0.015(3)
C21' 0.058(3) 0.064(3) 0.035(3) 0.015(2) 0.017(2) 0.015(3)
N2 0.0169(9) 0.0246(10) 0.0207(9) -0.0019(8) 0.0037(7) -0.0027(7)
C22 0.0183(10) 0.0285(12) 0.0217(11) -0.0041(9) -0.0006(9) -0.0020(9)
C23 0.0312(13) 0.0326(13) 0.0218(11) -0.0009(10) 0.0017(10) -0.0007(10)
C24 0.0376(15) 0.0419(15) 0.0269(13) 0.0016(12) -0.0010(11) 0.0059(12)
C25 0.067(2) 0.058(2) 0.0245(14) 0.0037(14) -0.0024(14) -0.0023(17)
C26 0.0200(11) 0.0231(11) 0.0189(10) -0.0018(9) 0.0031(8) -0.0044(9)
C27 0.0204(11) 0.0270(12) 0.0278(12) -0.0036(10) 0.0057(9) -0.0025(9)
C28 0.0260(12) 0.0280(12) 0.0320(13) -0.0065(10) 0.0017(10) -0.0008(10)
C29 0.0304(13) 0.0335(14) 0.0377(14) -0.0079(11) 0.0104(11) 0.0017(11)
C30 0.0185(10) 0.0261(12) 0.0239(11) 0.0000(9) 0.0055(9) -0.0041(9)
C31 0.0260(12) 0.0299(12) 0.0226(11) -0.0007(10) 0.0061(9) -0.0031(10)
C32 0.0507(18) 0.0382(15) 0.0301(14) 0.0011(12) 0.0090(13) -0.0151(13)
C33 0.0577(19) 0.0358(15) 0.0291(14) 0.0061(12) 0.0125(13) -0.0041(13)
C34 0.0152(10) 0.0273(12) 0.0240(11) -0.0006(9) 0.0041(8) -0.0003(9)
C35 0.0223(11) 0.0275(12) 0.0257(11) -0.0018(10) 0.0044(9) -0.0010(9)
C36 0.0264(13) 0.0312(13) 0.0346(14) 0.0001(11) 0.0101(10) 0.0022(10)
C37 0.0356(15) 0.0332(14) 0.0427(16) -0.0014(12) 0.0128(12) 0.0064(12)
N3 0.0437(15) 0.0414(15) 0.072(2) 0.0012(14) 0.0177(14) -0.0008(12)
C38 0.0320(14) 0.0409(16) 0.0390(15) 0.0023(13) 0.0075(12) -0.0067(12)
C39 0.0487(18) 0.0424(17) 0.0429(17) -0.0041(13) 0.0134(14) -0.0019(14)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 1.6509(18) . ?
Mo1 O2 2.0778(16) . ?
Mo1 O3 1.8017(18) . ?
Mo1 O4 2.0850(17) . ?
Mo1 O5 1.8071(18) . ?
Mo1 O6 2.2280(15) . ?
Mo2 O4 2.0614(16) . ?
Mo2 O6 2.2252(16) . ?
Mo2 O7 1.613(2) . ?
Mo2 O8 1.8300(17) . ?
Mo2 O9 1.8095(18) . ?
Mo2 O10 2.0558(16) . ?
Mo3 O2 2.0437(17) . ?
Mo3 O6 2.2384(15) . ?
Mo3 O10 2.0597(17) . ?
Mo3 O11 1.6192(18) . ?
Mo3 O12 1.7954(18) . ?
Mo3 O13 1.8428(18) . ?
Mo4 O6 2.3677(15) . ?
Mo4 O9 1.9621(19) . ?
Mo4 O13 1.8986(18) . ?
Mo4 O14 1.667(2) . ?
Mo4 O15 1.8769(19) . ?
Mo4 O16 1.9351(18) . ?
Mo5 O3 1.9468(18) . ?
Mo5 O6 2.3342(16) . ?
Mo5 O12 1.9390(18) . ?
Mo5 O15 1.8991(18) . ?
Mo5 O17 1.649(2) . ?
Mo5 O18 1.8806(18) . ?
Mo6 O5 1.9880(17) . ?
Mo6 O6 2.3454(15) . ?
Mo6 O8 1.9299(18) . ?
Mo6 O16 1.8655(19) . ?
Mo6 O18 1.9155(18) . ?
Mo6 O19 1.664(2) . ?
V1 O1 1.6509(18) . ?
V1 O2 2.0778(16) . ?
V1 O3 1.8017(18) . ?
V1 O4 2.0850(17) . ?
V1 O5 1.8071(18) . ?
V1 O6 2.2280(15) . ?
V2 O4 2.0614(16) . ?
V2 O6 2.2252(16) . ?
V2 O7 1.613(2) . ?
V2 O8 1.8300(17) . ?
V2 O9 1.8095(18) . ?
V2 O10 2.0558(16) . ?
V3 O2 2.0437(17) . ?
V3 O6 2.2384(15) . ?
V3 O10 2.0597(17) . ?
V3 O11 1.6192(18) . ?
V3 O12 1.7954(18) . ?
V3 O13 1.8428(18) . ?
V4 O6 2.3677(15) . ?
V4 O9 1.9621(19) . ?
V4 O13 1.8986(18) . ?
V4 O14 1.667(2) . ?
V4 O15 1.8769(19) . ?
V4 O16 1.9351(18) . ?
V5 O3 1.9468(18) . ?
V5 O6 2.3342(16) . ?
V5 O12 1.9390(18) . ?
V5 O15 1.8991(18) . ?
V5 O17 1.649(2) . ?
V5 O18 1.8806(18) . ?
V6 O5 1.9880(17) . ?
V6 O6 2.3454(15) . ?
V6 O8 1.9299(18) . ?
V6 O16 1.8655(19) . ?
V6 O18 1.9155(18) . ?
V6 O19 1.664(2) . ?
O2 C1 1.434(3) . ?
O4 C3 1.433(3) . ?
O10 C2 1.437(3) . ?
O20 H20 0.8200 . ?
O20 C5 1.421(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.527(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.525(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.522(3) . ?
C4 C5 1.536(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N1 C6 1.517(3) . ?
N1 C10 1.526(3) . ?
N1 C14 1.523(4) . ?
N1 C18 1.520(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.515(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.521(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.514(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.514(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.520(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.508(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.510(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.507(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.506(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C18 C19 1.548(7) . ?
C18 C19' 1.587(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.483(11) . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C19' C20' 1.545(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.406(9) . ?
C20' H20C 0.9700 . ?
C20' H20D 0.9700 . ?
C20' C21' 1.473(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21' H21D 0.9600 . ?
C21' H21E 0.9600 . ?
C21' H21F 0.9600 . ?
N2 C22 1.513(3) . ?
N2 C26 1.518(3) . ?
N2 C30 1.527(3) . ?
N2 C34 1.520(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.517(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.531(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.510(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.514(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.520(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.529(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.506(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.519(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.517(4) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.525(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.527(3) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.521(4) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
N3 C38 1.143(4) . ?
C38 C39 1.456(4) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
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 O2 95.02(8) . . ?
O1 Mo1 O3 106.51(9) . . ?
O1 Mo1 O4 94.54(8) . . ?
O1 Mo1 O5 105.76(9) . . ?
O1 Mo1 O6 167.29(8) . . ?
O2 Mo1 O4 79.71(7) . . ?
O2 Mo1 O6 75.87(6) . . ?
O3 Mo1 O2 87.23(7) . . ?
O3 Mo1 O4 156.13(7) . . ?
O3 Mo1 O5 97.03(8) . . ?
O3 Mo1 O6 82.19(7) . . ?
O4 Mo1 O6 75.31(6) . . ?
O5 Mo1 O2 156.50(7) . . ?
O5 Mo1 O4 87.69(7) . . ?
O5 Mo1 O6 81.81(7) . . ?
O4 Mo2 O6 75.84(6) . . ?
O7 Mo2 O4 95.34(8) . . ?
O7 Mo2 O6 169.32(8) . . ?
O7 Mo2 O8 104.47(9) . . ?
O7 Mo2 O9 105.77(9) . . ?
O7 Mo2 O10 96.88(8) . . ?
O8 Mo2 O4 86.61(7) . . ?
O8 Mo2 O6 81.29(7) . . ?
O8 Mo2 O10 156.29(8) . . ?
O9 Mo2 O4 157.32(8) . . ?
O9 Mo2 O6 82.24(7) . . ?
O9 Mo2 O8 95.85(8) . . ?
O9 Mo2 O10 88.03(7) . . ?
O10 Mo2 O4 81.19(6) . . ?
O10 Mo2 O6 76.06(6) . . ?
O2 Mo3 O6 76.31(6) . . ?
O2 Mo3 O10 81.60(7) . . ?
O10 Mo3 O6 75.69(6) . . ?
O11 Mo3 O2 95.44(8) . . ?
O11 Mo3 O6 169.64(8) . . ?
O11 Mo3 O10 97.12(8) . . ?
O11 Mo3 O12 104.87(9) . . ?
O11 Mo3 O13 105.78(9) . . ?
O12 Mo3 O2 88.72(8) . . ?
O12 Mo3 O6 81.48(7) . . ?
O12 Mo3 O10 156.72(7) . . ?
O12 Mo3 O13 95.29(8) . . ?
O13 Mo3 O2 156.52(7) . . ?
O13 Mo3 O6 81.42(7) . . ?
O13 Mo3 O10 85.83(7) . . ?
O9 Mo4 O6 75.56(6) . . ?
O13 Mo4 O6 76.92(6) . . ?
O13 Mo4 O9 86.76(8) . . ?
O13 Mo4 O16 153.16(8) . . ?
O14 Mo4 O6 177.73(9) . . ?
O14 Mo4 O9 102.23(9) . . ?
O14 Mo4 O13 103.54(10) . . ?
O14 Mo4 O15 104.45(9) . . ?
O14 Mo4 O16 103.08(10) . . ?
O15 Mo4 O6 77.75(7) . . ?
O15 Mo4 O9 153.23(8) . . ?
O15 Mo4 O13 89.13(8) . . ?
O15 Mo4 O16 87.56(8) . . ?
O16 Mo4 O6 76.36(7) . . ?
O16 Mo4 O9 84.34(8) . . ?
O3 Mo5 O6 76.52(6) . . ?
O12 Mo5 O3 84.91(8) . . ?
O12 Mo5 O6 76.16(7) . . ?
O15 Mo5 O3 154.62(8) . . ?
O15 Mo5 O6 78.21(7) . . ?
O15 Mo5 O12 86.83(8) . . ?
O17 Mo5 O3 102.05(9) . . ?
O17 Mo5 O6 177.32(9) . . ?
O17 Mo5 O12 101.51(9) . . ?
O17 Mo5 O15 103.10(9) . . ?
O17 Mo5 O18 103.82(9) . . ?
O18 Mo5 O3 87.78(8) . . ?
O18 Mo5 O6 78.47(7) . . ?
O18 Mo5 O12 154.58(8) . . ?
O18 Mo5 O15 89.49(8) . . ?
O5 Mo6 O6 75.27(6) . . ?
O8 Mo6 O5 83.87(7) . . ?
O8 Mo6 O6 76.21(6) . . ?
O16 Mo6 O5 153.44(8) . . ?
O16 Mo6 O6 78.18(7) . . ?
O16 Mo6 O8 89.13(8) . . ?
O16 Mo6 O18 89.93(8) . . ?
O18 Mo6 O5 85.16(7) . . ?
O18 Mo6 O6 77.53(6) . . ?
O18 Mo6 O8 153.34(7) . . ?
O19 Mo6 O5 102.86(9) . . ?
O19 Mo6 O6 178.07(9) . . ?
O19 Mo6 O8 103.18(9) . . ?
O19 Mo6 O16 103.67(10) . . ?
O19 Mo6 O18 102.92(9) . . ?
O1 V1 O2 95.02(8) . . ?
O1 V1 O3 106.51(9) . . ?
O1 V1 O4 94.54(8) . . ?
O1 V1 O5 105.76(9) . . ?
O1 V1 O6 167.29(8) . . ?
O2 V1 O4 79.71(7) . . ?
O2 V1 O6 75.87(6) . . ?
O3 V1 O2 87.23(7) . . ?
O3 V1 O4 156.13(7) . . ?
O3 V1 O5 97.03(8) . . ?
O3 V1 O6 82.19(7) . . ?
O4 V1 O6 75.31(6) . . ?
O5 V1 O2 156.50(7) . . ?
O5 V1 O4 87.69(7) . . ?
O5 V1 O6 81.81(7) . . ?
O4 V2 O6 75.84(6) . . ?
O7 V2 O4 95.34(8) . . ?
O7 V2 O6 169.32(8) . . ?
O7 V2 O8 104.47(9) . . ?
O7 V2 O9 105.77(9) . . ?
O7 V2 O10 96.88(8) . . ?
O8 V2 O4 86.61(7) . . ?
O8 V2 O6 81.29(7) . . ?
O8 V2 O10 156.29(8) . . ?
O9 V2 O4 157.32(8) . . ?
O9 V2 O6 82.24(7) . . ?
O9 V2 O8 95.85(8) . . ?
O9 V2 O10 88.03(7) . . ?
O10 V2 O4 81.19(6) . . ?
O10 V2 O6 76.06(6) . . ?
O2 V3 O6 76.31(6) . . ?
O2 V3 O10 81.60(7) . . ?
O10 V3 O6 75.69(6) . . ?
O11 V3 O2 95.44(8) . . ?
O11 V3 O6 169.64(8) . . ?
O11 V3 O10 97.12(8) . . ?
O11 V3 O12 104.87(9) . . ?
O11 V3 O13 105.78(9) . . ?
O12 V3 O2 88.72(8) . . ?
O12 V3 O6 81.48(7) . . ?
O12 V3 O10 156.72(7) . . ?
O12 V3 O13 95.29(8) . . ?
O13 V3 O2 156.52(7) . . ?
O13 V3 O6 81.42(7) . . ?
O13 V3 O10 85.83(7) . . ?
O9 V4 O6 75.56(6) . . ?
O13 V4 O6 76.92(6) . . ?
O13 V4 O9 86.76(8) . . ?
O13 V4 O16 153.16(8) . . ?
O14 V4 O6 177.73(9) . . ?
O14 V4 O9 102.23(9) . . ?
O14 V4 O13 103.54(10) . . ?
O14 V4 O15 104.45(9) . . ?
O14 V4 O16 103.08(10) . . ?
O15 V4 O6 77.75(7) . . ?
O15 V4 O9 153.23(8) . . ?
O15 V4 O13 89.13(8) . . ?
O15 V4 O16 87.56(8) . . ?
O16 V4 O6 76.36(7) . . ?
O16 V4 O9 84.34(8) . . ?
O3 V5 O6 76.52(6) . . ?
O12 V5 O3 84.91(8) . . ?
O12 V5 O6 76.16(7) . . ?
O15 V5 O3 154.62(8) . . ?
O15 V5 O6 78.21(7) . . ?
O15 V5 O12 86.83(8) . . ?
O17 V5 O3 102.05(9) . . ?
O17 V5 O6 177.32(9) . . ?
O17 V5 O12 101.51(9) . . ?
O17 V5 O15 103.10(9) . . ?
O17 V5 O18 103.82(9) . . ?
O18 V5 O3 87.78(8) . . ?
O18 V5 O6 78.47(7) . . ?
O18 V5 O12 154.58(8) . . ?
O18 V5 O15 89.49(8) . . ?
O5 V6 O6 75.27(6) . . ?
O8 V6 O5 83.87(7) . . ?
O8 V6 O6 76.21(6) . . ?
O16 V6 O5 153.44(8) . . ?
O16 V6 O6 78.18(7) . . ?
O16 V6 O8 89.13(8) . . ?
O16 V6 O18 89.93(8) . . ?
O18 V6 O5 85.16(7) . . ?
O18 V6 O6 77.53(6) . . ?
O18 V6 O8 153.34(7) . . ?
O19 V6 O5 102.86(9) . . ?
O19 V6 O6 178.07(9) . . ?
O19 V6 O8 103.18(9) . . ?
O19 V6 O16 103.67(10) . . ?
O19 V6 O18 102.92(9) . . ?
C1 O2 Mo1 120.24(14) . . ?
C1 O2 Mo3 118.97(14) . . ?
C1 O2 V1 120.24(14) . . ?
C1 O2 V3 118.97(14) . . ?
C3 O4 Mo1 120.45(14) . . ?
C3 O4 Mo2 117.93(13) . . ?
C3 O4 V1 120.45(14) . . ?
C3 O4 V2 117.93(13) . . ?
C2 O10 Mo2 119.31(14) . . ?
C2 O10 Mo3 118.17(14) . . ?
C2 O10 V2 119.31(14) . . ?
C2 O10 V3 118.17(14) . . ?
C5 O20 H20 109.5 . . ?
O2 C1 H1A 109.2 . . ?
O2 C1 H1B 109.2 . . ?
O2 C1 C4 112.07(19) . . ?
H1A C1 H1B 107.9 . . ?
C4 C1 H1A 109.2 . . ?
C4 C1 H1B 109.2 . . ?
O10 C2 H2A 109.1 . . ?
O10 C2 H2B 109.1 . . ?
O10 C2 C4 112.37(19) . . ?
H2A C2 H2B 107.9 . . ?
C4 C2 H2A 109.1 . . ?
C4 C2 H2B 109.1 . . ?
O4 C3 H3A 109.0 . . ?
O4 C3 H3B 109.0 . . ?
O4 C3 C4 113.07(19) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C1 C4 C5 107.8(2) . . ?
C2 C4 C1 110.8(2) . . ?
C2 C4 C5 108.5(2) . . ?
C3 C4 C1 110.5(2) . . ?
C3 C4 C2 109.9(2) . . ?
C3 C4 C5 109.3(2) . . ?
O20 C5 C4 112.8(2) . . ?
O20 C5 H5A 109.0 . . ?
O20 C5 H5B 109.0 . . ?
C4 C5 H5A 109.0 . . ?
C4 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
C6 N1 C10 111.6(2) . . ?
C6 N1 C14 107.87(19) . . ?
C6 N1 C18 108.8(2) . . ?
C14 N1 C10 109.1(2) . . ?
C18 N1 C10 108.2(2) . . ?
C18 N1 C14 111.3(2) . . ?
N1 C6 H6A 108.3 . . ?
N1 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
C7 C6 N1 116.0(2) . . ?
C7 C6 H6A 108.3 . . ?
C7 C6 H6B 108.3 . . ?
C6 C7 H7A 109.8 . . ?
C6 C7 H7B 109.8 . . ?
C6 C7 C8 109.3(2) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 C7 112.0(3) . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 H10A 108.4 . . ?
N1 C10 H10B 108.4 . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 N1 115.7(2) . . ?
C11 C10 H10A 108.4 . . ?
C11 C10 H10B 108.4 . . ?
C10 C11 H11A 109.8 . . ?
C10 C11 H11B 109.8 . . ?
C10 C11 C12 109.3(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
C11 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 C11 112.7(3) . . ?
C13 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 H14A 108.3 . . ?
N1 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
C15 C14 N1 115.8(2) . . ?
C15 C14 H14A 108.3 . . ?
C15 C14 H14B 108.3 . . ?
C14 C15 H15A 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 C14 109.8(2) . . ?
C16 C15 H15A 109.7 . . ?
C16 C15 H15B 109.7 . . ?
C15 C16 H16A 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C17 C16 C15 113.7(3) . . ?
C17 C16 H16A 108.8 . . ?
C17 C16 H16B 108.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 H18A 108.2 . . ?
N1 C18 H18B 108.2 . . ?
N1 C18 H18C 108.8 . . ?
N1 C18 H18D 108.8 . . ?
N1 C18 C19 113.7(3) . . ?
N1 C18 C19' 116.3(3) . . ?
H18A C18 H18B 107.4 . . ?
H18C C18 H18D 107.7 . . ?
C19 C18 H18C 108.8 . . ?
C19 C18 H18D 108.8 . . ?
C19' C18 H18A 108.2 . . ?
C19' C18 H18B 108.2 . . ?
C18 C19 H19A 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C20 C19 C18 111.0(5) . . ?
C20 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
C18 C19' H19C 109.9 . . ?
C18 C19' H19D 109.9 . . ?
H19C C19' H19D 108.3 . . ?
C20' C19' C18 109.0(5) . . ?
C20' C19' H19C 109.9 . . ?
C20' C19' H19D 109.9 . . ?
C19 C20 H20A 110.9 . . ?
C19 C20 H20B 110.9 . . ?
H20A C20 H20B 108.9 . . ?
C21 C20 C19 104.2(7) . . ?
C21 C20 H20A 110.9 . . ?
C21 C20 H20B 110.9 . . ?
C19' C20' H20C 107.7 . . ?
C19' C20' H20D 107.7 . . ?
H20C C20' H20D 107.1 . . ?
C21' C20' C19' 118.2(6) . . ?
C21' C20' H20C 107.7 . . ?
C21' C20' H20D 107.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20' C21' H21D 109.5 . . ?
C20' C21' H21E 109.5 . . ?
C20' C21' H21F 109.5 . . ?
H21D C21' H21E 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
C22 N2 C26 110.75(18) . . ?
C22 N2 C30 106.04(17) . . ?
C22 N2 C34 111.30(18) . . ?
C26 N2 C30 111.30(17) . . ?
C26 N2 C34 106.39(17) . . ?
C34 N2 C30 111.14(18) . . ?
N2 C22 H22A 108.0 . . ?
N2 C22 H22B 108.0 . . ?
N2 C22 C23 117.13(19) . . ?
H22A C22 H22B 107.3 . . ?
C23 C22 H22A 108.0 . . ?
C23 C22 H22B 108.0 . . ?
C22 C23 H23A 110.1 . . ?
C22 C23 H23B 110.1 . . ?
C22 C23 C24 108.1(2) . . ?
H23A C23 H23B 108.4 . . ?
C24 C23 H23A 110.1 . . ?
C24 C23 H23B 110.1 . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C25 C24 C23 112.9(3) . . ?
C25 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C26 H26A 108.6 . . ?
N2 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C27 C26 N2 114.71(19) . . ?
C27 C26 H26A 108.6 . . ?
C27 C26 H26B 108.6 . . ?
C26 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
C26 C27 C28 111.1(2) . . ?
H27A C27 H27B 108.0 . . ?
C28 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
C27 C28 H28A 109.4 . . ?
C27 C28 H28B 109.4 . . ?
C27 C28 C29 111.0(2) . . ?
H28A C28 H28B 108.0 . . ?
C29 C28 H28A 109.4 . . ?
C29 C28 H28B 109.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N2 C30 H30A 108.4 . . ?
N2 C30 H30B 108.4 . . ?
H30A C30 H30B 107.5 . . ?
C31 C30 N2 115.34(19) . . ?
C31 C30 H30A 108.4 . . ?
C31 C30 H30B 108.4 . . ?
C30 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
C30 C31 C32 111.5(2) . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
C31 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C33 C32 C31 111.6(2) . . ?
C33 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N2 C34 H34A 108.2 . . ?
N2 C34 H34B 108.2 . . ?
N2 C34 C35 116.37(19) . . ?
H34A C34 H34B 107.3 . . ?
C35 C34 H34A 108.2 . . ?
C35 C34 H34B 108.2 . . ?
C34 C35 H35A 109.8 . . ?
C34 C35 H35B 109.8 . . ?
C34 C35 C36 109.5(2) . . ?
H35A C35 H35B 108.2 . . ?
C36 C35 H35A 109.8 . . ?
C36 C35 H35B 109.8 . . ?
C35 C36 H36A 109.2 . . ?
C35 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
C37 C36 C35 112.0(2) . . ?
C37 C36 H36A 109.2 . . ?
C37 C36 H36B 109.2 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N3 C38 C39 179.3(4) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
_iucr_refine_instructions_details
;
hk-5-182.res created by SHELXL-2014/7
TITL hk-5-182_a.res in P2(1)/c
REM Old TITL HK-5-182 in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.142, Rweak 0.002, Alpha 0.059, Orientation as input
REM Formula found by SHELXT: C148 N12 O80 V12 Mo12
CELL 1.54184 15.7895 18.862 18.1257 90 98.459 90
ZERR 4 0.0002 0.0003 0.0002 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Mo N O V
UNIT 156 336 12 12 80 12
DFIX 1.5 C19 C21
DFIX 1.5 C21 C20
DFIX 1.5 C21' C20'
DFIX 1.5 C20' C19'
EADP Mo1 V1
EADP V2 Mo2
EADP V3 Mo3
EADP Mo4 V4
EADP Mo5 V5
EADP Mo6 V6
EADP C19' C19
EADP C21 C21'
EADP C20 C20'
EADP V1 Mo1
EADP Mo2 V2
EADP Mo3 V3
EADP V6 Mo6
EADP V5 Mo5
EADP V4 Mo4
EXYZ V1 Mo1
EXYZ Mo2 V2
EXYZ Mo3 V3
EXYZ V6 Mo6
EXYZ V5 Mo5
EXYZ V4 Mo4
L.S. 8
PLAN 20
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.041800 3.321400
FVAR 0.13529 0.53106
PART 16
MO1 3 0.811030 0.564695 0.642594 10.50000 0.01782 0.03038 =
0.02214 0.00187 0.00523 0.00005
PART 0
PART 17
MO2 3 0.751511 0.439403 0.757749 10.25000 0.01685 0.02279 =
0.02186 0.00093 0.00276 -0.00127
PART 0
PART 19
MO3 3 0.608823 0.559695 0.679081 10.25000 0.01339 0.02426 =
0.02426 -0.00130 0.00106 0.00087
PART 0
PART 26
MO4 3 0.678171 0.561455 0.851153 10.75000 0.02774 0.03527 =
0.02285 -0.00445 0.01026 -0.00392
PART 0
PART 24
MO5 3 0.738350 0.679889 0.741384 10.50000 0.01903 0.01762 =
0.03707 -0.00051 0.00001 -0.00154
PART 0
PART 22
MO6 3 0.875197 0.564740 0.817676 10.75000 0.01680 0.03200 =
0.02592 0.00074 -0.00297 -0.00290
PART 0
PART 15
V1 6 0.811030 0.564695 0.642594 10.50000 0.01782 0.03038 =
0.02214 0.00187 0.00523 0.00005
PART 0
PART 18
V2 6 0.751511 0.439403 0.757749 10.75000 0.01685 0.02279 =
0.02186 0.00093 0.00276 -0.00127
PART 0
PART 20
V3 6 0.608823 0.559695 0.679081 10.75000 0.01339 0.02426 =
0.02426 -0.00130 0.00106 0.00087
PART 0
PART 25
V4 6 0.678171 0.561455 0.851153 10.25000 0.02774 0.03527 =
0.02285 -0.00445 0.01026 -0.00392
PART 0
PART 23
V5 6 0.738350 0.679889 0.741384 10.50000 0.01903 0.01762 =
0.03707 -0.00051 0.00001 -0.00154
PART 0
PART 21
V6 6 0.875197 0.564740 0.817676 10.25000 0.01680 0.03200 =
0.02592 0.00074 -0.00297 -0.00290
PART 0
O1 5 0.848622 0.555880 0.562782 11.00000 0.02389 0.03674 =
0.02941 -0.00072 0.00728 -0.00260
O2 5 0.683562 0.551324 0.596519 11.00000 0.01810 0.02701 =
0.02108 0.00046 0.00188 0.00048
O3 5 0.787217 0.657435 0.651639 11.00000 0.02410 0.02633 =
0.03069 0.00437 0.00544 -0.00229
O4 5 0.797254 0.456039 0.658344 11.00000 0.01700 0.02309 =
0.02001 -0.00082 0.00362 -0.00067
O5 5 0.903409 0.561659 0.714387 11.00000 0.01670 0.02892 =
0.02629 -0.00228 0.00492 -0.00348
O6 5 0.742260 0.556185 0.741109 11.00000 0.01502 0.02377 =
0.01763 -0.00106 0.00381 -0.00128
O7 5 0.753859 0.354063 0.753144 11.00000 0.02600 0.03133 =
0.03638 0.00535 0.00528 0.00002
O8 5 0.858487 0.463997 0.803733 11.00000 0.01972 0.03048 =
0.02539 0.00378 -0.00230 -0.00008
O9 5 0.696960 0.459964 0.836191 11.00000 0.02575 0.03171 =
0.02406 0.00233 0.00541 -0.00322
O10 5 0.636624 0.453156 0.689545 11.00000 0.01564 0.02557 =
0.02130 -0.00263 0.00358 -0.00109
O11 5 0.518579 0.551877 0.624298 11.00000 0.01973 0.03708 =
0.03223 0.00051 0.00224 0.00320
O12 5 0.630258 0.653207 0.682836 11.00000 0.02093 0.02548 =
0.03559 -0.00023 0.00511 0.00508
O13 5 0.582631 0.553653 0.774654 11.00000 0.01729 0.03313 =
0.02891 -0.00567 0.00695 -0.00152
O14 5 0.634048 0.561804 0.929250 11.00000 0.04034 0.04687 =
0.03297 -0.00445 0.01494 -0.00899
O15 5 0.687263 0.657664 0.827060 11.00000 0.02364 0.02939 =
0.03352 -0.00754 0.00679 -0.00096
O16 5 0.799642 0.563188 0.887689 11.00000 0.02463 0.03822 =
0.02266 -0.00247 0.00023 -0.00513
O17 5 0.732777 0.767151 0.737717 11.00000 0.02716 0.02717 =
0.05910 -0.00275 0.00534 -0.00196
O18 5 0.846839 0.662061 0.796303 11.00000 0.02120 0.02783 =
0.02831 -0.00500 0.00333 -0.00430
O19 5 0.971116 0.569985 0.869566 11.00000 0.02726 0.04371 =
0.03700 0.00162 -0.00378 -0.00423
O20 5 0.653387 0.302296 0.518027 11.00000 0.03392 0.03587 =
0.05220 -0.01609 0.00752 -0.00329
AFIX 147
H20 2 0.701234 0.288063 0.512862 11.00000 -1.50000
AFIX 0
C1 1 0.660538 0.500898 0.537763 11.00000 0.02130 0.03468 =
0.01832 -0.00190 0.00098 0.00051
AFIX 23
H1A 2 0.695393 0.508942 0.498734 11.00000 -1.20000
H1B 2 0.601115 0.508001 0.516451 11.00000 -1.20000
AFIX 0
C2 1 0.616251 0.408934 0.624827 11.00000 0.01805 0.02818 =
0.02400 -0.00561 0.00108 -0.00196
AFIX 23
H2A 2 0.556771 0.416145 0.603751 11.00000 -1.20000
H2B 2 0.623165 0.359620 0.639672 11.00000 -1.20000
AFIX 0
C3 1 0.766184 0.410953 0.596598 11.00000 0.02126 0.02761 =
0.02372 -0.00500 0.00700 0.00068
AFIX 23
H3A 2 0.772640 0.361898 0.612494 11.00000 -1.20000
H3B 2 0.800898 0.418129 0.557303 11.00000 -1.20000
AFIX 0
C4 1 0.672743 0.424563 0.565384 11.00000 0.01897 0.02844 =
0.02283 -0.00361 0.00194 -0.00092
C5 1 0.645872 0.375261 0.498565 11.00000 0.02633 0.03938 =
0.02861 -0.01167 0.00141 -0.00218
AFIX 23
H5A 2 0.586939 0.385316 0.477750 11.00000 -1.20000
H5B 2 0.681291 0.385073 0.460345 11.00000 -1.20000
AFIX 0
N1 4 0.498083 0.831644 0.620588 11.00000 0.02461 0.03550 =
0.03100 0.00099 0.00789 0.00979
C6 1 0.418516 0.844831 0.564393 11.00000 0.02056 0.02860 =
0.03925 -0.00059 0.00501 0.00227
AFIX 23
H6A 2 0.402333 0.800606 0.538836 11.00000 -1.20000
H6B 2 0.372295 0.858142 0.591423 11.00000 -1.20000
AFIX 0
C7 1 0.426245 0.901185 0.506223 11.00000 0.02606 0.03089 =
0.03556 0.00060 0.00089 -0.00158
AFIX 23
H7A 2 0.470751 0.888132 0.477158 11.00000 -1.20000
H7B 2 0.441759 0.946150 0.530477 11.00000 -1.20000
AFIX 0
C8 1 0.341094 0.908382 0.455248 11.00000 0.03355 0.03439 =
0.05082 0.00233 -0.00917 -0.00115
AFIX 23
H8A 2 0.326885 0.863557 0.430230 11.00000 -1.20000
H8B 2 0.296532 0.919229 0.485066 11.00000 -1.20000
AFIX 0
C9 1 0.343542 0.965959 0.397394 11.00000 0.05713 0.04433 =
0.04889 0.00507 -0.01593 0.00509
AFIX 137
H9A 2 0.354227 1.010881 0.421895 11.00000 -1.50000
H9B 2 0.289582 0.967572 0.365169 11.00000 -1.50000
H9C 2 0.388371 0.955930 0.368436 11.00000 -1.50000
AFIX 0
C10 1 0.576613 0.819113 0.582271 11.00000 0.02120 0.03904 =
0.03119 -0.00170 0.00727 0.00646
AFIX 23
H10A 2 0.588840 0.862476 0.557068 11.00000 -1.20000
H10B 2 0.625182 0.809608 0.620349 11.00000 -1.20000
AFIX 0
C11 1 0.569142 0.759139 0.526183 11.00000 0.03252 0.03176 =
0.03823 -0.00049 0.01487 0.00553
AFIX 23
H11A 2 0.522210 0.768427 0.486476 11.00000 -1.20000
H11B 2 0.557373 0.715061 0.550310 11.00000 -1.20000
AFIX 0
C12 1 0.652416 0.752718 0.493958 11.00000 0.03842 0.04729 =
0.03798 -0.00040 0.01724 0.00562
AFIX 23
H12A 2 0.663186 0.796894 0.469560 11.00000 -1.20000
H12B 2 0.699112 0.745134 0.534333 11.00000 -1.20000
AFIX 0
C13 1 0.651038 0.692851 0.438624 11.00000 0.05961 0.04454 =
0.05904 -0.00564 0.03148 0.00947
AFIX 137
H13A 2 0.640305 0.648954 0.462408 11.00000 -1.50000
H13B 2 0.705328 0.690348 0.420880 11.00000 -1.50000
H13C 2 0.606602 0.701148 0.397368 11.00000 -1.50000
AFIX 0
C14 1 0.513188 0.896878 0.670282 11.00000 0.02799 0.04397 =
0.03508 -0.00818 0.00269 0.01198
AFIX 23
H14A 2 0.514155 0.938241 0.638618 11.00000 -1.20000
H14B 2 0.464921 0.902094 0.697336 11.00000 -1.20000
AFIX 0
C15 1 0.594321 0.896429 0.726013 11.00000 0.03284 0.06144 =
0.03360 -0.00598 0.00263 0.01707
AFIX 23
H15A 2 0.598999 0.851902 0.753083 11.00000 -1.20000
H15B 2 0.643594 0.900812 0.700070 11.00000 -1.20000
AFIX 0
C16 1 0.593100 0.957148 0.779928 11.00000 0.02921 0.06440 =
0.03358 -0.00817 0.00205 0.00658
AFIX 23
H16A 2 0.571891 0.999157 0.752333 11.00000 -1.20000
H16B 2 0.553498 0.945932 0.814391 11.00000 -1.20000
AFIX 0
C17 1 0.679443 0.973485 0.823915 11.00000 0.03458 0.08306 =
0.03512 -0.00117 -0.00063 0.00452
AFIX 137
H17A 2 0.702031 0.931660 0.849873 11.00000 -1.50000
H17B 2 0.673589 1.010369 0.859310 11.00000 -1.50000
H17C 2 0.717730 0.988838 0.790591 11.00000 -1.50000
AFIX 0
C18 1 0.483855 0.765887 0.665711 11.00000 0.04769 0.04489 =
0.04434 0.01540 0.02593 0.02028
PART 1
AFIX 23
H18A 2 0.529837 0.762997 0.707452 21.00000 -1.20000
H18B 2 0.488332 0.724620 0.634585 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H18C 2 0.539068 0.745863 0.685689 -21.00000 -1.20000
H18D 2 0.453278 0.730914 0.632720 -21.00000 -1.20000
AFIX 0
C19 1 0.432943 0.780291 0.730884 -21.00000 0.03514 0.04664 =
0.03603 0.00414 0.01528 0.00474
AFIX 23
H19A 2 0.462604 0.815753 0.763821 -21.00000 -1.20000
H19B 2 0.376811 0.798797 0.711287 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C19' 1 0.395465 0.761616 0.697334 21.00000 0.03514 0.04664 =
0.03603 0.00414 0.01528 0.00474
AFIX 23
H19C 2 0.386673 0.804657 0.724498 21.00000 -1.20000
H19D 2 0.348694 0.756947 0.656466 21.00000 -1.20000
AFIX 0
PART 0
PART 2
C20 1 0.423186 0.714533 0.773660 -21.00000 0.04635 0.05208 =
0.02409 -0.01224 0.00794 -0.01125
AFIX 23
H20A 2 0.478288 0.692267 0.789256 -21.00000 -1.20000
H20B 2 0.396491 0.724490 0.817435 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C20' 1 0.397121 0.696885 0.749753 21.00000 0.04635 0.05208 =
0.02409 -0.01224 0.00794 -0.01125
AFIX 23
H20C 2 0.340584 0.692142 0.764107 21.00000 -1.20000
H20D 2 0.406969 0.654988 0.721165 21.00000 -1.20000
AFIX 0
PART 0
PART 2
C21 1 0.370429 0.671026 0.723297 -21.00000 0.05833 0.06364 =
0.03516 0.01504 0.01709 0.01538
AFIX 137
H21A 2 0.321674 0.697699 0.700617 -21.00000 -1.50000
H21B 2 0.351475 0.631200 0.749518 -21.00000 -1.50000
H21C 2 0.402115 0.654475 0.685368 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C21' 1 0.459946 0.696363 0.818394 21.00000 0.05833 0.06364 =
0.03516 0.01504 0.01709 0.01538
AFIX 137
H21D 2 0.516049 0.705525 0.806156 21.00000 -1.50000
H21E 2 0.459386 0.650840 0.842003 21.00000 -1.50000
H21F 2 0.445354 0.732384 0.851767 21.00000 -1.50000
AFIX 0
PART 0
N2 4 0.962008 0.853473 0.833452 11.00000 0.01689 0.02462 =
0.02065 -0.00192 0.00372 -0.00268
C22 1 0.900576 0.853976 0.761061 11.00000 0.01834 0.02851 =
0.02167 -0.00410 -0.00057 -0.00204
AFIX 23
H22A 2 0.845288 0.869980 0.771785 11.00000 -1.20000
H22B 2 0.893508 0.805508 0.743333 11.00000 -1.20000
AFIX 0
C23 1 0.924726 0.899118 0.698113 11.00000 0.03125 0.03255 =
0.02184 -0.00094 0.00167 -0.00073
AFIX 23
H23A 2 0.974489 0.879268 0.680020 11.00000 -1.20000
H23B 2 0.938513 0.946900 0.715704 11.00000 -1.20000
AFIX 0
C24 1 0.848377 0.900416 0.635362 11.00000 0.03757 0.04192 =
0.02690 0.00161 -0.00098 0.00588
AFIX 23
H24A 2 0.833648 0.852120 0.620170 11.00000 -1.20000
H24B 2 0.799469 0.920984 0.654193 11.00000 -1.20000
AFIX 0
C25 1 0.865958 0.942173 0.568146 11.00000 0.06738 0.05832 =
0.02447 0.00369 -0.00244 -0.00229
AFIX 137
H25A 2 0.815160 0.943611 0.531851 11.00000 -1.50000
H25B 2 0.911302 0.919852 0.546769 11.00000 -1.50000
H25C 2 0.882586 0.989598 0.583094 11.00000 -1.50000
AFIX 0
C26 1 0.984015 0.928553 0.859722 11.00000 0.02000 0.02313 =
0.01894 -0.00179 0.00314 -0.00437
AFIX 23
H26A 2 1.021566 0.926302 0.907095 11.00000 -1.20000
H26B 2 1.015513 0.951225 0.824126 11.00000 -1.20000
AFIX 0
C27 1 0.907579 0.974341 0.869141 11.00000 0.02040 0.02699 =
0.02781 -0.00357 0.00566 -0.00247
AFIX 23
H27A 2 0.873857 0.951052 0.902665 11.00000 -1.20000
H27B 2 0.871742 0.980075 0.821249 11.00000 -1.20000
AFIX 0
C28 1 0.935774 1.046773 0.900262 11.00000 0.02601 0.02797 =
0.03196 -0.00648 0.00171 -0.00077
AFIX 23
H28A 2 0.971857 1.069096 0.868039 11.00000 -1.20000
H28B 2 0.969222 1.041194 0.949264 11.00000 -1.20000
AFIX 0
C29 1 0.858532 1.094217 0.906087 11.00000 0.03040 0.03354 =
0.03768 -0.00786 0.01042 0.00172
AFIX 137
H29A 2 0.827638 1.102480 0.857154 11.00000 -1.50000
H29B 2 0.877797 1.138644 0.928360 11.00000 -1.50000
H29C 2 0.821658 1.071319 0.936402 11.00000 -1.50000
AFIX 0
C30 1 0.916703 0.813232 0.889451 11.00000 0.01850 0.02612 =
0.02391 -0.00003 0.00546 -0.00406
AFIX 23
H30A 2 0.861472 0.835270 0.890927 11.00000 -1.20000
H30B 2 0.906216 0.765109 0.871541 11.00000 -1.20000
AFIX 0
C31 1 0.964267 0.810159 0.967738 11.00000 0.02602 0.02989 =
0.02261 -0.00070 0.00608 -0.00309
AFIX 23
H31A 2 0.972709 0.857919 0.987281 11.00000 -1.20000
H31B 2 1.020190 0.789125 0.966970 11.00000 -1.20000
AFIX 0
C32 1 0.915707 0.766974 1.018548 11.00000 0.05073 0.03821 =
0.03012 0.00105 0.00896 -0.01506
AFIX 23
H32A 2 0.858811 0.786711 1.017479 11.00000 -1.20000
H32B 2 0.909582 0.718640 1.000264 11.00000 -1.20000
AFIX 0
C33 1 0.961466 0.766616 1.098235 11.00000 0.05769 0.03581 =
0.02914 0.00614 0.01248 -0.00407
AFIX 137
H33A 2 1.016729 0.744974 1.099787 11.00000 -1.50000
H33B 2 0.928321 0.740202 1.129116 11.00000 -1.50000
H33C 2 0.968304 0.814446 1.116230 11.00000 -1.50000
AFIX 0
C34 1 1.046144 0.818075 0.823848 11.00000 0.01522 0.02732 =
0.02403 -0.00060 0.00411 -0.00033
AFIX 23
H34A 2 1.087164 0.827667 0.868027 11.00000 -1.20000
H34B 2 1.067592 0.840208 0.781967 11.00000 -1.20000
AFIX 0
C35 1 1.043174 0.738160 0.810995 11.00000 0.02232 0.02751 =
0.02572 -0.00181 0.00445 -0.00101
AFIX 23
H35A 2 0.999489 0.726881 0.769213 11.00000 -1.20000
H35B 2 1.028734 0.714325 0.854903 11.00000 -1.20000
AFIX 0
C36 1 1.130336 0.712603 0.794829 11.00000 0.02639 0.03124 =
0.03462 0.00011 0.01007 0.00222
AFIX 23
H36A 2 1.139719 0.730020 0.746332 11.00000 -1.20000
H36B 2 1.174837 0.732082 0.831881 11.00000 -1.20000
AFIX 0
C37 1 1.136853 0.632149 0.795783 11.00000 0.03559 0.03317 =
0.04268 -0.00137 0.01275 0.00635
AFIX 137
H37A 2 1.093105 0.612673 0.758977 11.00000 -1.50000
H37B 2 1.129466 0.614803 0.844221 11.00000 -1.50000
H37C 2 1.192102 0.618189 0.784754 11.00000 -1.50000
AFIX 0
N3 4 0.811180 0.230614 0.495568 11.00000 0.04370 0.04137 =
0.07160 0.00118 0.01769 -0.00077
C38 1 0.842942 0.178900 0.481368 11.00000 0.03196 0.04089 =
0.03903 0.00229 0.00752 -0.00669
C39 1 0.884023 0.113058 0.464205 11.00000 0.04868 0.04244 =
0.04293 -0.00409 0.01335 -0.00192
AFIX 137
H39A 2 0.905633 0.117930 0.417652 11.00000 -1.50000
H39B 2 0.843048 0.075149 0.460529 11.00000 -1.50000
H39C 2 0.930477 0.102676 0.503117 11.00000 -1.50000
AFIX 0
HKLF 4
REM hk-5-182_a.res in P2(1)/c
REM R1 = 0.0306 for 9257 Fo > 4sig(Fo) and 0.0370 for all 10668 data
REM 634 parameters refined using 4 restraints
END
WGHT 0.0418 3.3212
REM Highest difference peak 0.853, deepest hole -0.967, 1-sigma level 0.077
Q1 1 0.3632 0.6479 0.7123 11.00000 0.05 0.56
Q2 1 0.4535 0.7914 0.7393 11.00000 0.05 0.49
Q3 1 0.8549 0.6261 0.8087 11.00000 0.05 0.45
Q4 1 0.8144 0.6695 0.7902 11.00000 0.05 0.39
Q5 1 0.6670 0.6551 0.6997 11.00000 0.05 0.39
Q6 1 0.8205 0.4585 0.7965 11.00000 0.05 0.38
Q7 1 0.6961 0.5625 0.7280 11.00000 0.05 0.38
Q8 1 0.7992 0.5529 0.7672 11.00000 0.05 0.37
Q9 1 0.6283 0.6220 0.6813 11.00000 0.05 0.37
Q10 1 0.8101 0.6300 0.6563 11.00000 0.05 0.36
Q11 1 0.7422 0.6004 0.7451 11.00000 0.05 0.36
Q12 1 0.6867 0.4993 0.8406 11.00000 0.05 0.34
Q13 1 0.6640 0.3998 0.5370 11.00000 0.05 0.33
Q14 1 0.9387 0.5442 0.8618 11.00000 0.05 0.33
Q15 1 0.6164 0.5408 0.7975 11.00000 0.05 0.33
Q16 1 0.7822 0.6235 0.6452 11.00000 0.05 0.33
Q17 1 0.8593 0.5044 0.8139 11.00000 0.05 0.33
Q18 1 0.9318 0.5891 0.8717 11.00000 0.05 0.33
Q19 1 0.8746 0.5396 0.6913 11.00000 0.05 0.33
Q20 1 0.6264 0.5002 0.6867 11.00000 0.05 0.33
REM The information below was added by Olex2.
REM
REM R1 = 0.0306 for 9257 Fo > 4sig(Fo) and 0.0370 for all 22564 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.85, deepest hole -0.97
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0370
REM R1_gt = 0.0306
REM wR_ref = 0.0854
REM GOOF = 1.028
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 22564
REM Reflections_gt = 9257
REM Parameters = n/a
REM Hole = -0.97
REM Peak = 0.85
REM Flack = n/a
;
_olex2_date_sample_data_collection 2016-12-29
_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 1.524
_oxdiff_exptl_absorpt_empirical_full_min 0.751
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
#######################################################################
#
# 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_hk-6-42
_database_code_depnum_ccdc_archive 'CCDC 1553742'
_audit_update_record
;
2017-06-02 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_audit_creation_date 2017-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C7 H11 Mo3 O21 V3'
_chemical_formula_sum 'C39 H83 Mo3 N2 O21 V3'
_chemical_formula_weight 1356.71
_chemical_melting_point ?
_chemical_oxdiff_formula V3Mo3O22C38H83N2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.0687 2.1097 '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'
O O 0.0492 0.0322 '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'
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'
_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 21.4889(13)
_cell_length_b 22.7196(17)
_cell_length_c 24.1556(17)
_cell_angle_alpha 90.952(6)
_cell_angle_beta 93.807(5)
_cell_angle_gamma 91.862(5)
_cell_volume 11758.9(14)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 4129
_cell_measurement_temperature 130.00(10)
_cell_measurement_theta_max 70.5900
_cell_measurement_theta_min 4.0680
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 9.497
_exptl_absorpt_correction_T_max 0.591
_exptl_absorpt_correction_T_min 0.462
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.533
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 5552
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -7 -2 0.0643
8 -12 -2 0.0600
12 1 8 0.0773
-7 13 3 0.0545
10 -3 -12 0.0529
-4 3 15 0.0647
0 -13 -7 0.0504
-12 2 8 0.0659
3 -3 -15 0.0599
2 12 -9 0.0372
-1 -12 10 0.0485
12 1 7 0.0781
-12 1 -7 0.0869
_exptl_crystal_size_max 0.166
_exptl_crystal_size_mid 0.131
_exptl_crystal_size_min 0.09
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-11.7793 -6.8221 -2.3490 0.1157 0.4863 0.8661
8.0114 -12.2154 -2.2057 0.9006 0.2675 -0.3426
11.5968 1.0490 7.6610 -0.0096 -0.0020 -1.0000
-7.2245 12.6125 2.9144 -0.9241 -0.2744 0.2660
9.5976 -2.5996 -11.7633 0.7814 -0.5988 -0.1753
-3.9737 2.9467 14.9350 -0.7595 0.5825 -0.2896
-0.1388 -12.7912 -7.4963 0.8960 0.2656 0.3558
-12.4880 1.9648 7.6770 -0.6863 0.5256 0.5027
3.2159 -2.9454 -15.1040 0.7453 -0.5717 0.3430
1.9642 11.8645 -9.3009 -0.2314 -0.9655 0.1194
-1.0307 -11.6468 9.7787 0.2286 0.9536 -0.1959
12.1296 0.7225 6.7006 0.0534 -0.0399 -0.9978
-12.1511 1.0979 -6.7541 -0.1440 -0.0435 0.9886
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0673
_diffrn_reflns_av_unetI/netI 0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 43456
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full 50.435
_diffrn_reflns_theta_max 50.435
_diffrn_reflns_theta_min 3.510
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 130.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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 -115.00 -11.00 1.00 10.00 -- -40.81 -57.00 90.00 104
2 \w -50.00 35.00 1.00 10.00 -- -40.81 38.00-120.00 85
3 \w -96.00 -2.00 1.00 10.00 -- -40.81 125.00 -60.00 94
4 \w 77.00 173.00 1.00 30.00 -- 106.63 30.00 0.00 96
5 \w 134.00 178.00 1.00 30.00 -- 106.63 61.00 -60.00 44
6 \w 41.00 121.00 1.00 30.00 -- 106.63-125.00 0.00 80
7 \w 35.00 121.00 1.00 30.00 -- 106.63-125.00 150.00 86
8 \w 76.00 172.00 1.00 30.00 -- 106.63 61.00-150.00 96
9 \w 80.00 178.00 1.00 30.00 -- 106.63 45.00 -90.00 98
10 \w 78.00 112.00 1.00 30.00 -- 106.63 61.00 -60.00 34
11 \w 28.00 140.00 1.00 30.00 -- 106.63 -77.00 150.00 112
12 \w 32.00 118.00 1.00 30.00 -- 106.63 -61.00 -30.00 86
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0261578000
_diffrn_orient_matrix_UB_12 -0.0504428000
_diffrn_orient_matrix_UB_13 -0.0339398000
_diffrn_orient_matrix_UB_21 -0.0235859000
_diffrn_orient_matrix_UB_22 -0.0448756000
_diffrn_orient_matrix_UB_23 0.0415819000
_diffrn_orient_matrix_UB_31 -0.0626713000
_diffrn_orient_matrix_UB_32 -0.0067868000
_diffrn_orient_matrix_UB_33 -0.0347271000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 12691
_reflns_number_total 24359
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 50.38
_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 3.417
_refine_diff_density_min -1.934
_refine_diff_density_rms 0.198
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.281
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 918
_refine_ls_number_reflns 24359
_refine_ls_number_restraints 12
_refine_ls_R_factor_all 0.1909
_refine_ls_R_factor_gt 0.1501
_refine_ls_restrained_S_all 1.283
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3839
_refine_ls_wR_factor_ref 0.4348
_refine_special_details ', Solvent Mask (Olex2)'
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Shared sites
{Mo2, V2}
{V1, Mo1}
{V3, Mo3}
{V5, Mo5}
{V6, Mo6}
{V4, Mo4}
{Mo9, V9}
{V8, Mo8}
{Mo7, V7}
{Mo11, V11}
{Mo12, V12}
{Mo10, V10}
{V20, Mo20}
{Mo22, V22}
{Mo24, V24}
{V23, Mo23}
{V19, Mo19}
{Mo21, V21}
{V14, Mo14}
{V18, Mo18}
{V17, Mo17}
{V13, Mo13}
{V15, Mo15}
{V16, Mo16}
3. Restrained distances
C27-O84
1.22 with sigma of 0.02
C27-C28
1.45 with sigma of 0.02
C28-C27
1.45 with sigma of 0.01
Mo13-O43
2 with sigma of 0.02
Mo18-O43
2 with sigma of 0.02
C15-O41
1.4 with sigma of 0.02
Mo18-O52
2 with sigma of 0.02
O52-Mo17
2 with sigma of 0.02
O84-O83
2.3 with sigma of 0.04
O83-C28
2.35 with sigma of 0.04
O84-C28
2.35 with sigma of 0.04
4. Restrained planarity
O83, O84, C27, C28
with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(V2) = Uanis(Mo2)
Uanis(Mo2) = Uanis(V2)
Uanis(V1) = Uanis(Mo1)
Uanis(V3) = Uanis(Mo3)
Uanis(Mo6) = Uanis(V6)
Uanis(Mo4) = Uanis(V4)
Uanis(Mo5) = Uanis(V5)
Uanis(V5) = Uanis(Mo5)
Uanis(V6) = Uanis(Mo6)
Uanis(V4) = Uanis(Mo4)
Uanis(Mo8) = Uanis(V8)
Uanis(Mo9) = Uanis(V9)
Uanis(V8) = Uanis(Mo8)
Uanis(Mo7) = Uanis(V7)
Uanis(Mo11) = Uanis(V11)
Uanis(Mo12) = Uanis(V12)
Uanis(Mo10) = Uanis(V10)
Uanis(Mo23) = Uanis(V23)
Uanis(Mo19) = Uanis(V19)
Uanis(Mo20) = Uanis(V20)
Uanis(V20) = Uanis(Mo20)
Uanis(Mo22) = Uanis(V22)
Uanis(Mo24) = Uanis(V24)
Uanis(V23) = Uanis(Mo23)
Uanis(V19) = Uanis(Mo19)
Uanis(Mo21) = Uanis(V21)
Uanis(Mo17) = Uanis(V17)
Uanis(Mo18) = Uanis(V18)
Uanis(Mo13) = Uanis(V13)
Uanis(Mo14) = Uanis(V14)
Uanis(Mo15) = Uanis(V15)
Uanis(Mo16) = Uanis(V16)
Uanis(V14) = Uanis(Mo14)
Uanis(V18) = Uanis(Mo18)
Uanis(V17) = Uanis(Mo17)
Uanis(V13) = Uanis(Mo13)
Uanis(V15) = Uanis(Mo15)
Uanis(V16) = Uanis(Mo16)
6. Others
Fixed Sof: Mo1(0.25) Mo2(0.5) Mo3(0.25) Mo4(0.75) Mo5(0.5) Mo6(0.75) V1(0.75)
V2(0.5) V3(0.75) V4(0.25) V5(0.5) V6(0.25) Mo7(0.5) Mo8(0.25) Mo9(0.25)
Mo10(0.75) Mo11(0.75) Mo12(0.5) V7(0.5) V8(0.75) V9(0.75) V10(0.25) V11(0.25)
V12(0.5) Mo13(0.5) Mo14(0.5) Mo15(0.5) Mo16(0.5) Mo17(0.5) Mo18(0.5) V13(0.5)
V14(0.5) V15(0.5) V16(0.5) V17(0.5) V18(0.5) Mo19(0.5) Mo20(0.5) Mo21(0.5)
Mo22(0.5) Mo23(0.5) Mo24(0.5) V19(0.5) V20(0.5) V21(0.5) V22(0.5) V23(0.5)
V24(0.5)
Fixed Uiso: O39(0.1) O40(0.1) O41(0.1) O42(0.1) O43(0.1) O47(0.1) O49(0.1)
O50(0.1) O51(0.1) O52(0.1) O53(0.07) O55(0.1) O57(0.07) O81(0.1) O82(0.1)
C15(0.1) C16(0.1) C17(0.1) C18(0.1) C19(0.1) C20(0.1) C21(0.1) O83(0.1)
O84(0.1) C22(0.1) C23(0.1) C24(0.1) C25(0.1) C26(0.1) C27(0.1) C28(0.1)
7.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B),
C10(H10A,H10B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
C19(H19A,H19B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B)
7.b Idealised Me refined as rotating group:
C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C)
;
_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 0.10422(14) 0.67859(13) 0.55520(12) 0.0906(8) Uani 0.25 1 d . . P A 6
Mo2 Mo 0.16452(13) 0.74488(12) 0.44649(11) 0.1005(8) Uani 0.5 1 d . . P A 3
Mo3 Mo 0.25068(12) 0.73050(12) 0.56570(11) 0.0804(7) Uani 0.25 1 d . . P A 8
Mo4 Mo 0.13420(12) 0.60915(11) 0.44659(10) 0.1096(8) Uani 0.75 1 d . . P A 14
Mo5 Mo 0.21672(12) 0.59483(10) 0.56049(10) 0.0835(7) Uani 0.5 1 d . . P A 10
Mo6 Mo 0.27740(10) 0.65924(9) 0.45697(9) 0.0921(6) Uani 0.75 1 d . . P A 12
V1 V 0.10422(14) 0.67859(13) 0.55520(12) 0.0906(8) Uani 0.75 1 d . . P A 5
V2 V 0.16452(13) 0.74488(12) 0.44649(11) 0.1005(8) Uani 0.5 1 d . . P A 4
V3 V 0.25068(12) 0.73050(12) 0.56570(11) 0.0804(7) Uani 0.75 1 d . . P A 7
V4 V 0.13420(12) 0.60915(11) 0.44659(10) 0.1096(8) Uani 0.25 1 d . . P A 13
V5 V 0.21672(12) 0.59483(10) 0.56049(10) 0.0835(7) Uani 0.5 1 d . . P A 9
V6 V 0.27740(10) 0.65924(9) 0.45697(9) 0.0921(6) Uani 0.25 1 d . . P A 11
O1 O 0.0461(6) 0.6931(6) 0.5858(7) 0.111(5) Uani 1 1 d . . . . .
O2 O 0.1633(6) 0.7367(5) 0.5979(5) 0.081(4) Uani 1 1 d . . . . .
O3 O 0.0937(6) 0.7450(5) 0.5022(5) 0.084(3) Uani 1 1 d . . . . .
O4 O 0.1428(6) 0.6238(5) 0.5912(5) 0.084(4) Uani 1 1 d . . . . .
O5 O 0.0728(7) 0.6308(7) 0.5001(6) 0.104(5) Uani 1 1 d . . . . .
O6 O 0.1913(6) 0.6761(5) 0.5069(6) 0.085(4) Uani 1 1 d . . . . .
O7 O 0.1430(7) 0.8019(6) 0.4109(5) 0.096(4) Uani 1 1 d . . . . .
O8 O 0.2132(6) 0.7914(6) 0.5101(5) 0.079(3) Uani 1 1 d . . . . .
O9 O 0.1176(7) 0.6834(6) 0.4123(5) 0.088(4) Uani 1 1 d . . . . .
O10 O 0.2406(6) 0.7269(6) 0.4214(5) 0.084(3) Uani 1 1 d . . . . .
O11 O 0.2865(6) 0.7811(6) 0.6081(6) 0.089(4) Uani 1 1 d . . . . .
O12 O 0.2583(6) 0.6626(6) 0.5982(6) 0.093(4) Uani 1 1 d . . . . .
O13 O 0.3071(6) 0.7147(6) 0.5132(6) 0.096(4) Uani 1 1 d . . . . .
O14 O 0.0956(9) 0.5594(9) 0.4021(6) 0.145(7) Uani 1 1 d . . . . .
O15 O 0.2108(6) 0.6118(6) 0.4172(5) 0.092(4) Uani 1 1 d . . . . .
O16 O 0.1632(7) 0.5593(6) 0.5005(6) 0.108(5) Uani 1 1 d . . . . .
O17 O 0.3387(7) 0.6489(6) 0.4210(7) 0.113(5) Uani 1 1 d . . . . .
O18 O 0.2834(7) 0.6011(7) 0.5134(7) 0.124(6) Uani 1 1 d . . . . .
O19 O 0.2341(8) 0.5496(13) 0.5953(8) 0.178(11) Uani 1 1 d . . . . .
O77 O 0.0527(6) 0.8853(6) 0.6083(6) 0.088(4) Uani 1 1 d . . . . .
O78 O 0.0672(9) 0.9776(8) 0.6466(8) 0.126(6) Uani 1 1 d . . . . .
C1 C 0.0796(10) 0.8050(10) 0.5299(9) 0.099(7) Uani 1 1 d . . . . .
H1A H 0.0649 0.8314 0.5011 0.119 Uiso 1 1 calc R . . . .
H1B H 0.0459 0.7986 0.5542 0.119 Uiso 1 1 calc R . . . .
C2 C 0.1403(8) 0.7950(8) 0.6108(8) 0.083(6) Uani 1 1 d . . . . .
H2A H 0.1703 0.8155 0.6367 0.100 Uiso 1 1 calc R . . . .
H2B H 0.1015 0.7903 0.6288 0.100 Uiso 1 1 calc R . . . .
C3 C 0.1874(9) 0.8446(7) 0.5322(7) 0.073(5) Uani 1 1 d . . . . .
H3A H 0.1788 0.8715 0.5021 0.087 Uiso 1 1 calc R . . . .
H3B H 0.2181 0.8637 0.5585 0.087 Uiso 1 1 calc R . . . .
C4 C 0.1294(9) 0.8322(8) 0.5602(8) 0.080(5) Uani 1 1 d . . . . .
C5 C 0.1091(10) 0.8899(8) 0.5801(9) 0.088(6) Uani 1 1 d . . . . .
H5A H 0.1419 0.9077 0.6050 0.106 Uiso 1 1 calc R . . . .
H5B H 0.1028 0.9156 0.5486 0.106 Uiso 1 1 calc R . . . .
C6 C 0.0380(11) 0.9333(14) 0.6425(9) 0.107(8) Uani 1 1 d . . . . .
C7 C -0.0182(15) 0.9231(12) 0.6619(9) 0.140(11) Uani 1 1 d . . . . .
H7A H -0.0382 0.8894 0.6430 0.210 Uiso 1 1 calc GR . . . .
H7B H -0.0433 0.9569 0.6557 0.210 Uiso 1 1 calc GR . . . .
H7C H -0.0135 0.9159 0.7010 0.210 Uiso 1 1 calc GR . . . .
Mo7 Mo 0.27728(12) 0.06015(11) 0.53868(11) 0.0927(7) Uani 0.5 1 d . . P B 19
Mo8 Mo 0.23478(13) 0.19608(12) 0.57284(11) 0.0821(7) Uani 0.25 1 d . . P B 18
Mo9 Mo 0.22571(13) 0.15214(13) 0.44057(11) 0.0841(8) Uani 0.25 1 d . . P B 15
Mo10 Mo 0.32580(9) 0.24927(8) 0.48781(8) 0.0849(6) Uani 0.75 1 d . . P B 25
Mo11 Mo 0.36556(9) 0.11824(9) 0.45253(8) 0.0851(6) Uani 0.75 1 d . . P B 21
Mo12 Mo 0.37538(9) 0.15884(10) 0.58306(8) 0.0717(6) Uani 0.5 1 d . . P B 23
V7 V 0.27728(12) 0.06015(11) 0.53868(11) 0.0927(7) Uani 0.5 1 d . . P B 20
V8 V 0.23478(13) 0.19608(12) 0.57284(11) 0.0821(7) Uani 0.75 1 d . . P B 17
V9 V 0.22571(13) 0.15214(13) 0.44057(11) 0.0841(8) Uani 0.75 1 d . . P B 16
V10 V 0.32580(9) 0.24927(8) 0.48781(8) 0.0849(6) Uani 0.25 1 d . . P B 26
V11 V 0.36556(9) 0.11824(9) 0.45253(8) 0.0851(6) Uani 0.25 1 d . . P B 22
V12 V 0.37538(9) 0.15884(10) 0.58306(8) 0.0717(6) Uani 0.5 1 d . . P B 24
O20 O 0.2503(5) -0.0048(6) 0.5555(5) 0.082(3) Uani 1 1 d . . . . .
O21 O 0.2179(6) 0.1082(5) 0.5819(5) 0.074(3) Uani 1 1 d . . . . .
O22 O 0.3370(6) 0.0835(6) 0.5945(5) 0.085(3) Uani 1 1 d . . . . .
O23 O 0.3313(6) 0.0468(6) 0.4885(5) 0.090(4) Uani 1 1 d . . . . .
O24 O 0.2084(6) 0.0731(5) 0.4787(4) 0.069(3) Uani 1 1 d . . . . .
O25 O 0.2941(5) 0.1524(6) 0.5109(5) 0.084(4) Uani 1 1 d . . . . .
O26 O 0.1824(6) 0.2186(6) 0.6110(5) 0.085(3) Uani 1 1 d . . . . .
O27 O 0.1751(5) 0.1816(5) 0.5022(4) 0.065(3) Uani 1 1 d . . . . .
O28 O 0.3057(6) 0.1928(7) 0.6200(5) 0.095(4) Uani 1 1 d . . . . .
O29 O 0.2614(6) 0.2622(5) 0.5386(5) 0.089(4) Uani 1 1 d . . . . .
O30 O 0.1686(6) 0.1474(6) 0.3946(5) 0.091(4) Uani 1 1 d . . . . .
O31 O 0.2904(5) 0.1197(5) 0.4078(5) 0.075(3) Uani 1 1 d . . . . .
O32 O 0.2564(6) 0.2271(6) 0.4336(5) 0.082(3) Uani 1 1 d . . . . .
O33 O 0.3476(7) 0.3152(8) 0.4684(6) 0.111(5) Uani 1 1 d . . . . .
O34 O 0.3758(6) 0.2005(6) 0.4439(5) 0.089(4) Uani 1 1 d . . . . .
O35 O 0.3841(6) 0.2366(6) 0.5490(6) 0.088(4) Uani 1 1 d . . . . .
O36 O 0.4168(6) 0.1285(6) 0.5219(5) 0.086(4) Uani 1 1 d . . . . .
O37 O 0.4182(6) 0.0911(7) 0.4099(7) 0.110(5) Uani 1 1 d . . . . .
O38 O 0.4330(7) 0.1602(7) 0.6358(6) 0.112(5) Uani 1 1 d . . . . .
O79 O 0.0244(6) 0.0958(6) 0.5779(5) 0.083(4) Uani 1 1 d . . . . .
O80 O -0.0566(8) 0.0363(9) 0.5659(9) 0.158(10) Uani 1 1 d . . . . .
C8 C 0.1490(8) 0.0542(9) 0.4840(6) 0.074(5) Uani 1 1 d . . . . .
H8A H 0.1483 0.0133 0.4949 0.089 Uiso 1 1 calc R . . . .
H8B H 0.1252 0.0567 0.4486 0.089 Uiso 1 1 calc R . . . .
C9 C 0.1531(7) 0.0854(8) 0.5840(7) 0.068(5) Uani 1 1 d . . . . .
H9A H 0.1322 0.1072 0.6117 0.082 Uiso 1 1 calc R . . . .
H9B H 0.1530 0.0442 0.5941 0.082 Uiso 1 1 calc R . . . .
C10 C 0.1182(8) 0.1541(10) 0.5089(7) 0.086(6) Uani 1 1 d . . . . .
H10A H 0.0936 0.1550 0.4738 0.103 Uiso 1 1 calc R . . . .
H10B H 0.0968 0.1770 0.5356 0.103 Uiso 1 1 calc R . . . .
C11 C 0.1194(9) 0.0918(8) 0.5277(7) 0.071(5) Uani 1 1 d . . . . .
C12 C 0.0511(10) 0.0675(9) 0.5351(9) 0.095(7) Uani 1 1 d . . . . .
H12A H 0.0257 0.0725 0.5009 0.114 Uiso 1 1 calc R . . . .
H12B H 0.0521 0.0257 0.5424 0.114 Uiso 1 1 calc R . . . .
C13 C -0.0266(14) 0.0702(17) 0.5912(11) 0.122(13) Uani 1 1 d . . . . .
C14 C -0.0437(15) 0.0959(15) 0.6294(19) 0.22(2) Uani 1 1 d . . . . .
H14A H -0.0831 0.1130 0.6193 0.324 Uiso 1 1 calc GR . . . .
H14B H -0.0136 0.1266 0.6409 0.324 Uiso 1 1 calc GR . . . .
H14C H -0.0486 0.0693 0.6594 0.324 Uiso 1 1 calc GR . . . .
Mo13 Mo 0.3421(2) 0.2157(3) -0.05646(17) 0.1880(19) Uani 0.5 1 d D . P C 46
Mo14 Mo 0.3761(4) 0.1422(3) 0.0637(2) 0.240(3) Uani 0.5 1 d . . P C 40
Mo15 Mo 0.2640(4) 0.2326(4) 0.0566(2) 0.263(3) Uani 0.5 1 d . . P C 48
Mo16 Mo 0.2365(5) 0.1008(3) 0.06239(17) 0.310(5) Uani 0.5 1 d . . P C 50
Mo17 Mo 0.1994(2) 0.1697(2) -0.05057(13) 0.1643(16) Uani 0.5 1 d D . P C 44
Mo18 Mo 0.3121(3) 0.08277(18) -0.04557(14) 0.1783(19) Uani 0.5 1 d D . P C 42
V13 V 0.3421(2) 0.2157(3) -0.05646(17) 0.1880(19) Uani 0.5 1 d . . P C 45
V14 V 0.3761(4) 0.1422(3) 0.0637(2) 0.240(3) Uani 0.5 1 d . . P C 39
V15 V 0.2640(4) 0.2326(4) 0.0566(2) 0.263(3) Uani 0.5 1 d . . P C 47
V16 V 0.2365(5) 0.1008(3) 0.06239(17) 0.310(5) Uani 0.5 1 d . . P C 49
V17 V 0.1994(2) 0.1697(2) -0.05057(13) 0.1643(16) Uani 0.5 1 d . . P C 43
V18 V 0.3121(3) 0.08277(18) -0.04557(14) 0.1783(19) Uani 0.5 1 d . . P C 41
O39 O 0.3863(7) 0.2624(6) -0.0928(6) 0.100 Uiso 1 1 d . . . . .
O40 O 0.2608(7) 0.2174(6) -0.0784(6) 0.100 Uiso 1 1 d . . . . .
O41 O 0.3141(7) 0.2739(6) -0.0006(6) 0.100 Uiso 1 1 d D . . . .
O42 O 0.4064(7) 0.2053(6) 0.0055(6) 0.100 Uiso 1 1 d . . . . .
O43 O 0.3848(6) 0.1402(5) -0.0342(6) 0.100 Uiso 1 1 d D . . . .
O44 O 0.2991(7) 0.1617(7) 0.0078(7) 0.111(5) Uiso 1 1 d . . . . .
O45 O 0.4402(12) 0.1462(11) 0.1016(11) 0.187(9) Uiso 1 1 d . . . . .
O46 O 0.3437(10) 0.2222(9) 0.0876(9) 0.148(7) Uiso 1 1 d . . . . .
O47 O 0.2476(7) 0.2968(6) 0.0911(6) 0.100 Uiso 1 1 d . . . . .
O48 O 0.1993(11) 0.2286(10) -0.0012(10) 0.164(8) Uiso 1 1 d . . . . .
O49 O 0.2273(7) 0.1706(7) 0.0672(6) 0.100 Uiso 1 1 d . . . . .
O50 O 0.1377(7) 0.1848(6) -0.0962(6) 0.100 Uiso 1 1 d . . . . .
O51 O 0.1733(7) 0.1216(6) 0.0082(6) 0.100 Uiso 1 1 d . . . . .
O52 O 0.2374(6) 0.1007(6) -0.0845(6) 0.100 Uiso 1 1 d D . . . .
O53 O 0.3308(5) 0.0219(5) -0.0790(5) 0.070 Uiso 1 1 d . . . . .
O54 O 0.2859(13) 0.0432(12) 0.0142(12) 0.200(10) Uiso 1 1 d . . . . .
O55 O 0.1970(7) 0.0538(6) 0.1020(6) 0.100 Uiso 1 1 d . . . . .
O56 O 0.3228(11) 0.0890(10) 0.0798(9) 0.150(7) Uiso 1 1 d . . . . .
O57 O 0.3804(5) 0.0868(5) 0.0143(5) 0.070 Uiso 1 1 d . . . . .
O81 O 0.4288(7) 0.3921(6) 0.1075(6) 0.100 Uiso 1 1 d . . . . .
O82 O 0.5181(7) 0.4233(6) 0.1481(6) 0.100 Uiso 1 1 d . . . . .
C15 C 0.3535(9) 0.3219(8) 0.0131(9) 0.100 Uiso 1 1 d D . . . .
H15A H 0.3304 0.3530 0.0293 0.120 Uiso 1 1 calc R . . . .
H15B H 0.3714 0.3368 -0.0200 0.120 Uiso 1 1 calc R . . . .
C16 C 0.4466(10) 0.2515(9) 0.0259(9) 0.100 Uiso 1 1 d . . . . .
H16A H 0.4624 0.2720 -0.0054 0.120 Uiso 1 1 calc R . . . .
H16B H 0.4819 0.2348 0.0464 0.120 Uiso 1 1 calc R . . . .
C17 C 0.3843(10) 0.2712(10) 0.1048(9) 0.100 Uiso 1 1 d . . . . .
H17A H 0.3595 0.3008 0.1214 0.120 Uiso 1 1 calc R . . . .
H17B H 0.4140 0.2580 0.1336 0.120 Uiso 1 1 calc R . . . .
C18 C 0.4175(10) 0.2979(10) 0.0644(10) 0.100 Uiso 1 1 d . . . . .
C19 C 0.4649(10) 0.3576(9) 0.0792(10) 0.100 Uiso 1 1 d . . . . .
H19A H 0.5020 0.3473 0.1015 0.120 Uiso 1 1 calc R . . . .
H19B H 0.4772 0.3763 0.0456 0.120 Uiso 1 1 calc R . . . .
C20 C 0.4600(11) 0.4257(10) 0.1374(10) 0.100 Uiso 1 1 d . . . . .
C21 C 0.4315(10) 0.4677(9) 0.1693(9) 0.100 Uiso 1 1 d . . . . .
H21A H 0.4026 0.4891 0.1459 0.150 Uiso 1 1 calc GR . . . .
H21B H 0.4628 0.4946 0.1864 0.150 Uiso 1 1 calc GR . . . .
H21C H 0.4095 0.4484 0.1976 0.150 Uiso 1 1 calc GR . . . .
Mo19 Mo 0.2683(3) 0.5986(3) 0.07435(19) 0.212(2) Uani 0.5 1 d . . P D 36
Mo20 Mo 0.2124(2) 0.5702(2) -0.05547(15) 0.1670(17) Uani 0.5 1 d . . P D 28
Mo21 Mo 0.3062(2) 0.6875(2) -0.02712(17) 0.1684(16) Uani 0.5 1 d . . P D 37
Mo22 Mo 0.16464(18) 0.70140(18) -0.06047(13) 0.1359(11) Uani 0.5 1 d . . P D 29
Mo23 Mo 0.2193(2) 0.72780(19) 0.06623(15) 0.1499(13) Uani 0.5 1 d . . P D 34
Mo24 Mo 0.12430(19) 0.6163(2) 0.03764(16) 0.1524(14) Uani 0.5 1 d . . P D 31
V19 V 0.2683(3) 0.5986(3) 0.07435(19) 0.212(2) Uani 0.5 1 d . . P D 35
V20 V 0.2124(2) 0.5702(2) -0.05547(15) 0.1670(17) Uani 0.5 1 d . . P D 27
V21 V 0.3062(2) 0.6875(2) -0.02712(17) 0.1684(16) Uani 0.5 1 d . . P D 38
V22 V 0.16464(18) 0.70140(18) -0.06047(13) 0.1359(11) Uani 0.5 1 d . . P D 30
V23 V 0.2193(2) 0.72780(19) 0.06623(15) 0.1499(13) Uani 0.5 1 d . . P D 33
V24 V 0.12430(19) 0.6163(2) 0.03764(16) 0.1524(14) Uani 0.5 1 d . . P D 32
O58 O 0.3085(12) 0.5592(11) 0.1156(11) 0.180(9) Uiso 1 1 d . . . . .
O59 O 0.1815(8) 0.5726(7) 0.0782(7) 0.121(5) Uiso 1 1 d . . . . .
O60 O 0.2550(9) 0.5423(8) 0.0031(8) 0.134(6) Uiso 1 1 d . . . . .
O61 O 0.3293(11) 0.6410(10) 0.0316(10) 0.167(8) Uiso 1 1 d . . . . .
O62 O 0.2593(9) 0.6823(9) 0.1000(8) 0.141(6) Uiso 1 1 d . . . . .
O63 O 0.2231(8) 0.6462(7) 0.0078(7) 0.122(5) Uiso 1 1 d . . . . .
O64 O 0.2119(10) 0.5163(9) -0.0919(9) 0.151(7) Uiso 1 1 d . . . . .
O65 O 0.2908(8) 0.6098(7) -0.0707(7) 0.120(5) Uiso 1 1 d . . . . .
O66 O 0.1752(9) 0.6287(8) -0.0966(8) 0.137(6) Uiso 1 1 d . . . . .
O67 O 0.1289(11) 0.5616(10) -0.0160(10) 0.166(8) Uiso 1 1 d . . . . .
O68 O 0.3760(12) 0.7059(11) -0.0573(10) 0.181(9) Uiso 1 1 d . . . . .
O69 O 0.2522(11) 0.7132(10) -0.0783(10) 0.170(8) Uiso 1 1 d . . . . .
O70 O 0.2985(11) 0.7366(10) 0.0324(10) 0.171(8) Uiso 1 1 d . . . . .
O71 O 0.1277(15) 0.7330(14) -0.1158(13) 0.240(13) Uiso 1 1 d . . . . .
O72 O 0.1751(12) 0.7533(11) 0.0029(11) 0.188(9) Uiso 1 1 d . . . . .
O73 O 0.1046(12) 0.6601(11) -0.0264(11) 0.182(9) Uiso 1 1 d . . . . .
O74 O 0.2242(13) 0.7858(13) 0.1096(12) 0.213(11) Uiso 1 1 d . . . . .
O75 O 0.1519(6) 0.6849(6) 0.0775(6) 0.089(4) Uiso 1 1 d . . . . .
O76 O 0.0531(11) 0.5955(11) 0.0607(10) 0.179(9) Uiso 1 1 d . . . . .
O83 O 0.3926(6) 0.4595(6) -0.0789(6) 0.100 Uiso 1 1 d D . . . .
O84 O 0.4265(6) 0.3976(6) -0.1498(6) 0.100 Uiso 1 1 d D . . . .
C22 C 0.3774(10) 0.5933(9) 0.0227(10) 0.100 Uiso 1 1 d . . . . .
H22A H 0.4164 0.6134 0.0152 0.120 Uiso 1 1 calc R . . . .
H22B H 0.3845 0.5733 0.0576 0.120 Uiso 1 1 calc R . . . .
C23 C 0.3038(10) 0.5042(10) -0.0032(10) 0.100 Uiso 1 1 d . . . . .
H23A H 0.2924 0.4748 -0.0320 0.120 Uiso 1 1 calc R . . . .
H23B H 0.3144 0.4844 0.0312 0.120 Uiso 1 1 calc R . . . .
C24 C 0.3418(10) 0.5735(10) -0.0840(9) 0.100 Uiso 1 1 d . . . . .
H24A H 0.3750 0.5966 -0.0993 0.120 Uiso 1 1 calc R . . . .
H24B H 0.3280 0.5419 -0.1099 0.120 Uiso 1 1 calc R . . . .
C25 C 0.3643(11) 0.5473(10) -0.0212(10) 0.100 Uiso 1 1 d . . . . .
C26 C 0.4250(10) 0.5039(9) -0.0321(9) 0.100 Uiso 1 1 d . . . . .
H26A H 0.4600 0.5261 -0.0456 0.120 Uiso 1 1 calc R . . . .
H26B H 0.4387 0.4833 0.0012 0.120 Uiso 1 1 calc R . . . .
C27 C 0.4417(9) 0.4299(7) -0.1117(7) 0.100 Uiso 1 1 d D . . . .
C28 C 0.4960(8) 0.4447(9) -0.0757(8) 0.100 Uiso 1 1 d D . . . .
H28A H 0.5080 0.4853 -0.0803 0.150 Uiso 1 1 calc GR . . . .
H28B H 0.5295 0.4202 -0.0849 0.150 Uiso 1 1 calc GR . . . .
H28C H 0.4867 0.4385 -0.0379 0.150 Uiso 1 1 calc GR . . . .
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 0.097(2) 0.0910(18) 0.0828(19) -0.0209(15) 0.0179(15) -0.0210(15)
Mo2 0.1123(19) 0.1131(19) 0.0757(16) -0.0141(14) 0.0128(13) -0.0089(14)
Mo3 0.0831(17) 0.0918(17) 0.0653(16) -0.0162(13) 0.0089(13) -0.0104(13)
Mo4 0.1203(18) 0.1152(17) 0.0907(16) -0.0352(13) 0.0118(13) -0.0261(13)
Mo5 0.1069(17) 0.0750(13) 0.0695(15) -0.0046(11) 0.0143(13) -0.0002(12)
Mo6 0.1009(14) 0.0986(13) 0.0786(13) -0.0205(11) 0.0293(11) -0.0036(11)
V1 0.097(2) 0.0910(18) 0.0828(19) -0.0209(15) 0.0179(15) -0.0210(15)
V2 0.1123(19) 0.1131(19) 0.0757(16) -0.0141(14) 0.0128(13) -0.0089(14)
V3 0.0831(17) 0.0918(17) 0.0653(16) -0.0162(13) 0.0089(13) -0.0104(13)
V4 0.1203(18) 0.1152(17) 0.0907(16) -0.0352(13) 0.0118(13) -0.0261(13)
V5 0.1069(17) 0.0750(13) 0.0695(15) -0.0046(11) 0.0143(13) -0.0002(12)
V6 0.1009(14) 0.0986(13) 0.0786(13) -0.0205(11) 0.0293(11) -0.0036(11)
O1 0.082(9) 0.099(10) 0.152(14) -0.035(10) 0.022(9) -0.017(7)
O2 0.094(9) 0.085(8) 0.064(7) -0.029(6) 0.027(6) -0.031(7)
O3 0.091(9) 0.082(8) 0.080(9) 0.006(7) 0.013(7) 0.001(6)
O4 0.100(9) 0.082(8) 0.068(8) -0.017(6) 0.016(7) -0.019(7)
O5 0.097(10) 0.129(11) 0.085(9) -0.041(9) 0.032(8) -0.048(8)
O6 0.084(8) 0.069(7) 0.100(10) -0.003(7) -0.001(7) 0.005(6)
O7 0.135(12) 0.086(9) 0.068(8) -0.002(7) 0.013(8) 0.009(8)
O8 0.084(8) 0.096(9) 0.055(7) -0.002(6) 0.008(6) -0.007(7)
O9 0.120(10) 0.091(9) 0.053(7) -0.010(6) 0.005(7) -0.014(7)
O10 0.105(9) 0.097(9) 0.053(7) -0.001(6) 0.012(6) 0.021(7)
O11 0.077(8) 0.091(8) 0.097(10) -0.027(7) 0.009(7) -0.008(6)
O12 0.097(9) 0.083(8) 0.098(10) -0.028(7) 0.000(8) 0.013(7)
O13 0.078(8) 0.118(10) 0.094(10) -0.044(8) 0.042(7) -0.017(7)
O14 0.157(15) 0.191(17) 0.080(10) -0.087(11) 0.007(10) -0.068(13)
O15 0.101(10) 0.108(10) 0.066(8) -0.021(7) 0.015(7) -0.010(7)
O16 0.122(11) 0.095(9) 0.105(11) -0.056(9) 0.026(9) -0.029(8)
O17 0.103(10) 0.109(10) 0.129(13) -0.030(9) 0.054(9) -0.016(8)
O18 0.110(11) 0.123(12) 0.142(14) -0.059(11) 0.051(10) -0.009(9)
O19 0.095(12) 0.34(3) 0.098(13) -0.085(17) 0.045(10) -0.021(16)
O77 0.086(9) 0.089(9) 0.090(9) -0.019(8) 0.028(7) -0.014(7)
O78 0.128(13) 0.110(12) 0.140(15) -0.041(11) 0.038(11) -0.026(10)
C1 0.081(14) 0.121(17) 0.100(16) -0.002(14) 0.033(12) 0.003(12)
C2 0.061(11) 0.088(13) 0.100(15) -0.049(12) 0.019(10) -0.007(9)
C3 0.107(14) 0.067(11) 0.045(10) -0.002(8) 0.007(9) -0.005(10)
C4 0.081(13) 0.079(12) 0.077(13) 0.000(11) -0.008(11) -0.012(10)
C5 0.101(15) 0.073(12) 0.090(15) 0.003(11) 0.009(12) 0.004(10)
C6 0.087(16) 0.16(2) 0.078(15) 0.000(16) 0.035(13) -0.002(16)
C7 0.20(3) 0.15(2) 0.063(15) -0.015(15) -0.005(18) -0.04(2)
Mo7 0.0963(17) 0.0993(16) 0.0825(16) -0.0094(13) 0.0089(13) 0.0020(13)
Mo8 0.0814(17) 0.0959(18) 0.0687(17) -0.0136(14) 0.0095(13) -0.0019(13)
Mo9 0.0886(18) 0.106(2) 0.0575(15) -0.0088(14) 0.0085(13) 0.0059(15)
Mo10 0.0918(13) 0.0843(12) 0.0800(13) -0.0076(10) 0.0203(10) -0.0035(10)
Mo11 0.0816(12) 0.1038(14) 0.0714(12) -0.0152(10) 0.0180(10) 0.0080(10)
Mo12 0.0638(12) 0.0968(14) 0.0532(12) -0.0115(10) 0.0007(9) -0.0045(10)
V7 0.0963(17) 0.0993(16) 0.0825(16) -0.0094(13) 0.0089(13) 0.0020(13)
V8 0.0814(17) 0.0959(18) 0.0687(17) -0.0136(14) 0.0095(13) -0.0019(13)
V9 0.0886(18) 0.106(2) 0.0575(15) -0.0088(14) 0.0085(13) 0.0059(15)
V10 0.0918(13) 0.0843(12) 0.0800(13) -0.0076(10) 0.0203(10) -0.0035(10)
V11 0.0816(12) 0.1038(14) 0.0714(12) -0.0152(10) 0.0180(10) 0.0080(10)
V12 0.0638(12) 0.0968(14) 0.0532(12) -0.0115(10) 0.0007(9) -0.0045(10)
O20 0.072(8) 0.100(9) 0.075(8) -0.006(7) 0.011(6) 0.016(6)
O21 0.090(9) 0.081(8) 0.053(7) -0.004(6) 0.013(6) 0.004(6)
O22 0.085(8) 0.095(9) 0.074(8) 0.010(7) 0.000(6) 0.004(7)
O23 0.085(9) 0.115(10) 0.074(8) 0.003(7) 0.020(7) 0.017(7)
O24 0.089(9) 0.076(7) 0.041(6) -0.010(5) 0.011(6) -0.006(6)
O25 0.055(7) 0.118(10) 0.078(8) -0.013(7) 0.018(6) -0.016(6)
O26 0.087(8) 0.096(9) 0.071(8) -0.016(7) 0.009(6) -0.005(7)
O27 0.065(7) 0.086(7) 0.044(6) -0.009(5) 0.008(5) 0.010(6)
O28 0.068(8) 0.152(12) 0.066(8) -0.022(8) 0.013(6) 0.008(7)
O29 0.106(10) 0.086(8) 0.078(9) -0.015(7) 0.046(7) 0.001(7)
O30 0.101(9) 0.121(10) 0.054(7) -0.013(7) 0.013(7) 0.017(8)
O31 0.059(7) 0.085(8) 0.082(8) -0.007(6) 0.006(6) 0.008(6)
O32 0.077(8) 0.110(9) 0.059(7) 0.004(7) 0.000(6) 0.001(7)
O33 0.111(11) 0.155(14) 0.067(9) -0.014(9) 0.011(8) 0.013(10)
O34 0.090(9) 0.099(9) 0.080(9) -0.022(7) 0.038(7) 0.000(7)
O35 0.075(8) 0.098(9) 0.090(9) -0.006(8) -0.007(7) 0.006(6)
O36 0.073(8) 0.111(10) 0.073(8) -0.014(7) -0.006(6) 0.005(7)
O37 0.084(9) 0.122(11) 0.132(13) -0.025(10) 0.057(9) 0.014(8)
O38 0.089(10) 0.158(14) 0.082(10) -0.017(9) -0.031(8) -0.014(9)
O79 0.088(10) 0.109(9) 0.056(7) -0.024(7) 0.031(7) 0.009(7)
O80 0.114(13) 0.177(18) 0.181(19) -0.120(16) 0.067(12) -0.074(13)
C8 0.083(13) 0.101(13) 0.037(9) -0.024(9) -0.008(8) 0.016(10)
C9 0.050(9) 0.092(12) 0.064(11) -0.006(9) 0.020(8) -0.016(8)
C10 0.052(11) 0.17(2) 0.035(9) -0.026(11) -0.017(8) 0.013(11)
C11 0.091(13) 0.081(12) 0.042(10) 0.005(9) 0.011(9) 0.000(10)
C12 0.104(16) 0.091(14) 0.082(15) -0.011(12) -0.035(13) 0.000(12)
C13 0.087(19) 0.21(3) 0.073(16) -0.035(18) 0.045(14) 0.04(2)
C14 0.12(3) 0.17(3) 0.34(6) 0.13(4) -0.08(3) -0.10(3)
Mo13 0.197(4) 0.260(6) 0.109(3) -0.033(3) 0.020(3) 0.030(4)
Mo14 0.306(8) 0.270(7) 0.140(4) -0.053(4) -0.048(5) 0.101(6)
Mo15 0.274(8) 0.359(10) 0.157(5) -0.081(5) 0.041(5) 0.009(7)
Mo16 0.545(14) 0.304(8) 0.073(3) -0.049(4) 0.082(5) -0.192(9)
Mo17 0.230(4) 0.191(4) 0.074(2) -0.026(2) 0.012(2) 0.053(3)
Mo18 0.311(6) 0.149(3) 0.074(2) -0.011(2) 0.002(3) 0.028(3)
V13 0.197(4) 0.260(6) 0.109(3) -0.033(3) 0.020(3) 0.030(4)
V14 0.306(8) 0.270(7) 0.140(4) -0.053(4) -0.048(5) 0.101(6)
V15 0.274(8) 0.359(10) 0.157(5) -0.081(5) 0.041(5) 0.009(7)
V16 0.545(14) 0.304(8) 0.073(3) -0.049(4) 0.082(5) -0.192(9)
V17 0.230(4) 0.191(4) 0.074(2) -0.026(2) 0.012(2) 0.053(3)
V18 0.311(6) 0.149(3) 0.074(2) -0.011(2) 0.002(3) 0.028(3)
Mo19 0.244(6) 0.287(7) 0.105(3) -0.022(4) 0.009(3) 0.027(5)
Mo20 0.206(4) 0.201(4) 0.091(2) -0.025(2) 0.017(2) -0.047(3)
Mo21 0.179(4) 0.202(4) 0.123(3) -0.002(3) 0.024(3) -0.033(3)
Mo22 0.150(3) 0.168(3) 0.090(2) -0.008(2) 0.0043(18) 0.018(2)
Mo23 0.172(3) 0.171(3) 0.105(2) -0.035(2) 0.011(2) 0.003(3)
Mo24 0.146(3) 0.195(4) 0.117(3) -0.026(3) 0.031(2) -0.023(3)
V19 0.244(6) 0.287(7) 0.105(3) -0.022(4) 0.009(3) 0.027(5)
V20 0.206(4) 0.201(4) 0.091(2) -0.025(2) 0.017(2) -0.047(3)
V21 0.179(4) 0.202(4) 0.123(3) -0.002(3) 0.024(3) -0.033(3)
V22 0.150(3) 0.168(3) 0.090(2) -0.008(2) 0.0043(18) 0.018(2)
V23 0.172(3) 0.171(3) 0.105(2) -0.035(2) 0.011(2) 0.003(3)
V24 0.146(3) 0.195(4) 0.117(3) -0.026(3) 0.031(2) -0.023(3)
_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 O1 1.535(15) . ?
Mo1 O2 2.023(11) . ?
Mo1 O3 2.004(12) . ?
Mo1 O4 1.734(14) . ?
Mo1 O5 1.786(12) . ?
Mo1 O6 2.271(13) . ?
Mo2 O3 2.098(13) . ?
Mo2 O6 2.219(13) . ?
Mo2 O7 1.630(13) . ?
Mo2 O8 2.058(12) . ?
Mo2 O9 1.846(12) . ?
Mo2 O10 1.837(13) . ?
Mo3 O2 2.087(12) . ?
Mo3 O6 2.185(12) . ?
Mo3 O8 2.087(13) . ?
Mo3 O11 1.663(12) . ?
Mo3 O12 1.749(14) . ?
Mo3 O13 1.850(11) . ?
Mo4 O5 1.976(13) . ?
Mo4 O6 2.346(12) . ?
Mo4 O9 1.926(13) . ?
Mo4 O14 1.703(12) . ?
Mo4 O15 1.835(13) . ?
Mo4 O16 1.831(18) . ?
Mo5 O4 1.926(13) . ?
Mo5 O6 2.331(13) . ?
Mo5 O12 1.938(13) . ?
Mo5 O16 1.937(14) . ?
Mo5 O18 1.890(15) . ?
Mo5 O19 1.38(3) . ?
Mo6 O6 2.314(13) . ?
Mo6 O10 1.939(12) . ?
Mo6 O13 1.901(12) . ?
Mo6 O15 1.953(13) . ?
Mo6 O17 1.646(14) . ?
Mo6 O18 1.92(2) . ?
V1 O1 1.535(15) . ?
V1 O2 2.023(11) . ?
V1 O3 2.004(12) . ?
V1 O4 1.734(14) . ?
V1 O5 1.786(12) . ?
V1 O6 2.271(13) . ?
V2 O3 2.098(13) . ?
V2 O6 2.219(13) . ?
V2 O7 1.630(13) . ?
V2 O8 2.058(12) . ?
V2 O9 1.846(12) . ?
V2 O10 1.837(13) . ?
V3 O2 2.087(12) . ?
V3 O6 2.185(12) . ?
V3 O8 2.087(13) . ?
V3 O11 1.663(12) . ?
V3 O12 1.749(14) . ?
V3 O13 1.850(11) . ?
V4 O5 1.976(13) . ?
V4 O6 2.346(12) . ?
V4 O9 1.926(13) . ?
V4 O14 1.703(12) . ?
V4 O15 1.835(13) . ?
V4 O16 1.831(18) . ?
V5 O4 1.926(13) . ?
V5 O6 2.331(13) . ?
V5 O12 1.938(13) . ?
V5 O16 1.937(14) . ?
V5 O18 1.890(15) . ?
V5 O19 1.38(3) . ?
V6 O6 2.314(13) . ?
V6 O10 1.939(12) . ?
V6 O13 1.901(12) . ?
V6 O15 1.953(13) . ?
V6 O17 1.646(14) . ?
V6 O18 1.92(2) . ?
O2 C2 1.47(2) . ?
O3 C1 1.55(2) . ?
O8 C3 1.45(2) . ?
O77 C5 1.43(2) . ?
O77 C6 1.41(3) . ?
O78 C6 1.17(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.38(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.51(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.48(3) . ?
C4 C5 1.48(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.34(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
Mo7 O20 1.635(13) . ?
Mo7 O21 2.035(11) . ?
Mo7 O22 1.856(12) . ?
Mo7 O23 1.762(12) . ?
Mo7 O24 2.034(12) . ?
Mo7 O25 2.236(13) . ?
Mo8 O21 2.035(12) . ?
Mo8 O25 2.265(12) . ?
Mo8 O26 1.592(13) . ?
Mo8 O27 2.080(10) . ?
Mo8 O28 1.846(13) . ?
Mo8 O29 1.822(13) . ?
Mo9 O24 2.066(11) . ?
Mo9 O25 2.171(12) . ?
Mo9 O27 2.019(10) . ?
Mo9 O30 1.599(13) . ?
Mo9 O31 1.815(11) . ?
Mo9 O32 1.821(13) . ?
Mo10 O25 2.370(13) . ?
Mo10 O29 1.936(11) . ?
Mo10 O32 1.965(12) . ?
Mo10 O33 1.639(17) . ?
Mo10 O34 1.922(12) . ?
Mo10 O35 1.905(12) . ?
Mo11 O23 1.997(14) . ?
Mo11 O25 2.298(12) . ?
Mo11 O31 1.885(11) . ?
Mo11 O34 1.891(13) . ?
Mo11 O36 1.950(12) . ?
Mo11 O37 1.703(12) . ?
Mo12 O22 1.909(13) . ?
Mo12 O25 2.383(12) . ?
Mo12 O28 1.966(12) . ?
Mo12 O35 1.969(13) . ?
Mo12 O36 1.904(13) . ?
Mo12 O38 1.714(12) . ?
V7 O20 1.635(13) . ?
V7 O21 2.035(11) . ?
V7 O22 1.856(12) . ?
V7 O23 1.762(12) . ?
V7 O24 2.034(12) . ?
V7 O25 2.236(13) . ?
V8 O21 2.035(12) . ?
V8 O25 2.265(12) . ?
V8 O26 1.592(13) . ?
V8 O27 2.080(10) . ?
V8 O28 1.846(13) . ?
V8 O29 1.822(13) . ?
V9 O24 2.066(11) . ?
V9 O25 2.171(12) . ?
V9 O27 2.019(10) . ?
V9 O30 1.599(13) . ?
V9 O31 1.815(11) . ?
V9 O32 1.821(13) . ?
V10 O25 2.370(13) . ?
V10 O29 1.936(11) . ?
V10 O32 1.965(12) . ?
V10 O33 1.639(17) . ?
V10 O34 1.922(12) . ?
V10 O35 1.905(12) . ?
V11 O23 1.997(14) . ?
V11 O25 2.298(12) . ?
V11 O31 1.885(11) . ?
V11 O34 1.891(13) . ?
V11 O36 1.950(12) . ?
V11 O37 1.703(12) . ?
V12 O22 1.909(13) . ?
V12 O25 2.383(12) . ?
V12 O28 1.966(12) . ?
V12 O35 1.969(13) . ?
V12 O36 1.904(13) . ?
V12 O38 1.714(12) . ?
O21 C9 1.474(19) . ?
O24 C8 1.35(2) . ?
O27 C10 1.38(2) . ?
O79 C12 1.38(2) . ?
O79 C13 1.29(4) . ?
O80 C13 1.13(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C11 1.53(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C11 1.51(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.50(3) . ?
C11 C12 1.57(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.17(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
Mo13 O39 1.696(15) . ?
Mo13 O40 1.794(15) . ?
Mo13 O41 2.007(15) . ?
Mo13 O42 1.991(15) . ?
Mo13 O43 2.034(12) . ?
Mo13 O44 2.224(16) . ?
Mo14 O42 2.140(16) . ?
Mo14 O43 2.385(16) . ?
Mo14 O44 2.127(16) . ?
Mo14 O45 1.60(3) . ?
Mo14 O46 2.05(2) . ?
Mo14 O56 1.70(2) . ?
Mo14 O57 1.728(12) . ?
Mo15 O41 2.030(16) . ?
Mo15 O44 2.167(17) . ?
Mo15 O46 1.85(2) . ?
Mo15 O47 1.726(15) . ?
Mo15 O48 1.90(2) . ?
Mo15 O49 1.625(15) . ?
Mo16 O44 2.376(17) . ?
Mo16 O49 1.609(16) . ?
Mo16 O51 1.899(16) . ?
Mo16 O54 2.10(3) . ?
Mo16 O55 1.691(15) . ?
Mo16 O56 1.90(2) . ?
Mo17 O40 1.848(15) . ?
Mo17 O44 2.499(16) . ?
Mo17 O48 1.78(2) . ?
Mo17 O50 1.716(15) . ?
Mo17 O51 1.909(15) . ?
Mo17 O52 1.981(12) . ?
Mo18 O43 2.004(12) . ?
Mo18 O44 2.226(16) . ?
Mo18 O52 1.866(12) . ?
Mo18 O53 1.663(12) . ?
Mo18 O54 1.82(3) . ?
Mo18 O57 1.990(12) . ?
V13 O39 1.696(15) . ?
V13 O40 1.794(15) . ?
V13 O41 2.007(15) . ?
V13 O42 1.991(15) . ?
V13 O43 2.034(12) . ?
V13 O44 2.224(16) . ?
V14 O42 2.140(16) . ?
V14 O43 2.385(16) . ?
V14 O44 2.127(16) . ?
V14 O45 1.60(3) . ?
V14 O46 2.05(2) . ?
V14 O56 1.70(2) . ?
V14 O57 1.728(12) . ?
V15 O41 2.030(16) . ?
V15 O44 2.167(17) . ?
V15 O46 1.85(2) . ?
V15 O47 1.726(15) . ?
V15 O48 1.90(2) . ?
V15 O49 1.625(15) . ?
V16 O44 2.376(17) . ?
V16 O49 1.609(16) . ?
V16 O51 1.899(16) . ?
V16 O54 2.10(3) . ?
V16 O55 1.691(15) . ?
V16 O56 1.90(2) . ?
V17 O40 1.848(15) . ?
V17 O48 1.78(2) . ?
V17 O50 1.716(15) . ?
V17 O51 1.909(15) . ?
V17 O52 1.981(12) . ?
V18 O43 2.004(12) . ?
V18 O44 2.226(16) . ?
V18 O52 1.866(12) . ?
V18 O53 1.663(12) . ?
V18 O54 1.82(3) . ?
V18 O57 1.990(12) . ?
O41 C15 1.381(15) . ?
O42 O43 1.782(19) . ?
O42 C16 1.40(2) . ?
O43 O57 1.707(16) . ?
O46 C17 1.43(3) . ?
O81 C19 1.33(2) . ?
O81 C20 1.20(2) . ?
O82 C20 1.26(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C18 1.89(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C18 1.57(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.38(3) . ?
C18 C19 1.69(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.40(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
Mo19 O58 1.58(3) . ?
Mo19 O59 1.948(18) . ?
Mo19 O60 2.13(2) . ?
Mo19 O61 1.96(2) . ?
Mo19 O62 2.01(2) . ?
Mo19 O63 2.149(18) . ?
Mo20 O60 1.771(19) . ?
Mo20 O63 2.282(18) . ?
Mo20 O64 1.50(2) . ?
Mo20 O65 1.944(17) . ?
Mo20 O66 1.844(19) . ?
Mo20 O67 2.09(2) . ?
Mo21 O61 1.84(2) . ?
Mo21 O63 2.212(17) . ?
Mo21 O65 2.048(17) . ?
Mo21 O68 1.75(3) . ?
Mo21 O69 1.76(2) . ?
Mo21 O70 1.82(2) . ?
Mo22 O63 2.400(18) . ?
Mo22 O66 1.882(19) . ?
Mo22 O69 1.97(2) . ?
Mo22 O71 1.69(3) . ?
Mo22 O72 1.91(3) . ?
Mo22 O73 1.82(3) . ?
Mo23 O62 1.57(2) . ?
Mo23 O63 2.318(18) . ?
Mo23 O70 1.94(2) . ?
Mo23 O72 1.86(3) . ?
Mo23 O74 1.66(3) . ?
Mo23 O75 1.759(13) . ?
Mo24 O59 1.847(17) . ?
Mo24 O63 2.370(18) . ?
Mo24 O67 1.79(2) . ?
Mo24 O73 1.89(3) . ?
Mo24 O75 1.876(13) . ?
Mo24 O76 1.72(2) . ?
V19 O58 1.58(3) . ?
V19 O59 1.948(18) . ?
V19 O60 2.13(2) . ?
V19 O61 1.96(2) . ?
V19 O62 2.01(2) . ?
V19 O63 2.149(18) . ?
V20 O60 1.771(19) . ?
V20 O63 2.282(18) . ?
V20 O64 1.50(2) . ?
V20 O65 1.944(17) . ?
V20 O66 1.844(19) . ?
V20 O67 2.09(2) . ?
V21 O61 1.84(2) . ?
V21 O63 2.212(17) . ?
V21 O65 2.048(17) . ?
V21 O68 1.75(3) . ?
V21 O69 1.76(2) . ?
V21 O70 1.82(2) . ?
V22 O63 2.400(18) . ?
V22 O66 1.882(19) . ?
V22 O69 1.97(2) . ?
V22 O71 1.69(3) . ?
V22 O72 1.91(3) . ?
V22 O73 1.82(3) . ?
V23 O62 1.57(2) . ?
V23 O63 2.318(18) . ?
V23 O70 1.94(2) . ?
V23 O72 1.86(3) . ?
V23 O74 1.66(3) . ?
V23 O75 1.759(13) . ?
V24 O59 1.847(17) . ?
V24 O63 2.370(18) . ?
V24 O67 1.79(2) . ?
V24 O73 1.89(3) . ?
V24 O75 1.876(13) . ?
V24 O76 1.72(2) . ?
O60 C23 1.40(3) . ?
O61 C22 1.54(3) . ?
O65 C24 1.44(3) . ?
O83 C26 1.61(2) . ?
O83 C27 1.53(2) . ?
O84 C27 1.189(15) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C25 1.48(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C25 1.69(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.69(3) . ?
C25 C26 1.69(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.434(9) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
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 O2 96.5(6) . . ?
O1 Mo1 O3 93.9(8) . . ?
O1 Mo1 O4 108.0(8) . . ?
O1 Mo1 O5 102.4(7) . . ?
O1 Mo1 O6 168.9(7) . . ?
O2 Mo1 O6 77.2(5) . . ?
O3 Mo1 O2 83.5(6) . . ?
O3 Mo1 O6 76.5(5) . . ?
O4 Mo1 O2 86.8(6) . . ?
O4 Mo1 O3 156.9(6) . . ?
O4 Mo1 O5 94.9(7) . . ?
O4 Mo1 O6 81.0(5) . . ?
O5 Mo1 O2 159.5(5) . . ?
O5 Mo1 O3 87.2(7) . . ?
O5 Mo1 O6 82.8(5) . . ?
O3 Mo2 O6 75.9(5) . . ?
O7 Mo2 O3 97.7(6) . . ?
O7 Mo2 O6 170.7(6) . . ?
O7 Mo2 O8 96.4(6) . . ?
O7 Mo2 O9 103.4(7) . . ?
O7 Mo2 O10 104.7(7) . . ?
O8 Mo2 O3 82.4(5) . . ?
O8 Mo2 O6 76.3(5) . . ?
O9 Mo2 O3 84.3(6) . . ?
O9 Mo2 O6 82.8(5) . . ?
O9 Mo2 O8 157.5(5) . . ?
O10 Mo2 O3 156.2(5) . . ?
O10 Mo2 O6 80.9(5) . . ?
O10 Mo2 O8 87.0(5) . . ?
O10 Mo2 O9 98.2(6) . . ?
O2 Mo3 O6 77.9(5) . . ?
O2 Mo3 O8 82.0(5) . . ?
O8 Mo3 O6 76.5(5) . . ?
O11 Mo3 O2 95.8(5) . . ?
O11 Mo3 O6 169.7(6) . . ?
O11 Mo3 O8 94.7(6) . . ?
O11 Mo3 O12 107.0(7) . . ?
O11 Mo3 O13 105.2(6) . . ?
O12 Mo3 O2 88.5(6) . . ?
O12 Mo3 O6 81.2(6) . . ?
O12 Mo3 O8 157.1(6) . . ?
O12 Mo3 O13 94.5(7) . . ?
O13 Mo3 O2 156.9(5) . . ?
O13 Mo3 O6 80.0(5) . . ?
O13 Mo3 O8 86.6(6) . . ?
O5 Mo4 O6 77.1(5) . . ?
O9 Mo4 O5 86.4(6) . . ?
O9 Mo4 O6 77.8(5) . . ?
O14 Mo4 O5 105.1(7) . . ?
O14 Mo4 O6 177.6(8) . . ?
O14 Mo4 O9 103.2(8) . . ?
O14 Mo4 O15 100.0(7) . . ?
O14 Mo4 O16 99.6(9) . . ?
O15 Mo4 O5 154.9(5) . . ?
O15 Mo4 O6 77.8(5) . . ?
O15 Mo4 O9 88.3(6) . . ?
O16 Mo4 O5 84.9(7) . . ?
O16 Mo4 O6 79.5(5) . . ?
O16 Mo4 O9 157.0(5) . . ?
O16 Mo4 O15 90.6(7) . . ?
O4 Mo5 O6 75.7(5) . . ?
O4 Mo5 O12 84.6(5) . . ?
O4 Mo5 O16 88.0(6) . . ?
O12 Mo5 O6 73.7(5) . . ?
O16 Mo5 O6 77.9(6) . . ?
O16 Mo5 O12 151.6(7) . . ?
O18 Mo5 O4 152.4(7) . . ?
O18 Mo5 O6 77.0(7) . . ?
O18 Mo5 O12 83.8(6) . . ?
O18 Mo5 O16 90.6(7) . . ?
O19 Mo5 O4 103.7(8) . . ?
O19 Mo5 O6 175.6(9) . . ?
O19 Mo5 O12 101.9(9) . . ?
O19 Mo5 O16 106.5(10) . . ?
O19 Mo5 O18 103.2(9) . . ?
O10 Mo6 O6 76.5(5) . . ?
O10 Mo6 O15 86.7(6) . . ?
O13 Mo6 O6 75.6(5) . . ?
O13 Mo6 O10 84.5(6) . . ?
O13 Mo6 O15 152.0(5) . . ?
O13 Mo6 O18 86.4(7) . . ?
O15 Mo6 O6 76.5(5) . . ?
O17 Mo6 O6 178.6(7) . . ?
O17 Mo6 O10 102.3(7) . . ?
O17 Mo6 O13 103.7(6) . . ?
O17 Mo6 O15 104.1(7) . . ?
O17 Mo6 O18 104.2(8) . . ?
O18 Mo6 O6 77.0(5) . . ?
O18 Mo6 O10 153.4(6) . . ?
O18 Mo6 O15 89.8(6) . . ?
O1 V1 O2 96.5(6) . . ?
O1 V1 O3 93.9(8) . . ?
O1 V1 O4 108.0(8) . . ?
O1 V1 O5 102.4(7) . . ?
O1 V1 O6 168.9(7) . . ?
O2 V1 O6 77.2(5) . . ?
O3 V1 O2 83.5(6) . . ?
O3 V1 O6 76.5(5) . . ?
O4 V1 O2 86.8(6) . . ?
O4 V1 O3 156.9(6) . . ?
O4 V1 O5 94.9(7) . . ?
O4 V1 O6 81.0(5) . . ?
O5 V1 O2 159.5(5) . . ?
O5 V1 O3 87.2(7) . . ?
O5 V1 O6 82.8(5) . . ?
O3 V2 O6 75.9(5) . . ?
O7 V2 O3 97.7(6) . . ?
O7 V2 O6 170.7(6) . . ?
O7 V2 O8 96.4(6) . . ?
O7 V2 O9 103.4(7) . . ?
O7 V2 O10 104.7(7) . . ?
O8 V2 O3 82.4(5) . . ?
O8 V2 O6 76.3(5) . . ?
O9 V2 O3 84.3(6) . . ?
O9 V2 O6 82.8(5) . . ?
O9 V2 O8 157.5(5) . . ?
O10 V2 O3 156.2(5) . . ?
O10 V2 O6 80.9(5) . . ?
O10 V2 O8 87.0(5) . . ?
O10 V2 O9 98.2(6) . . ?
O2 V3 O6 77.9(5) . . ?
O2 V3 O8 82.0(5) . . ?
O8 V3 O6 76.5(5) . . ?
O11 V3 O2 95.8(5) . . ?
O11 V3 O6 169.7(6) . . ?
O11 V3 O8 94.7(6) . . ?
O11 V3 O12 107.0(7) . . ?
O11 V3 O13 105.2(6) . . ?
O12 V3 O2 88.5(6) . . ?
O12 V3 O6 81.2(6) . . ?
O12 V3 O8 157.1(6) . . ?
O12 V3 O13 94.5(7) . . ?
O13 V3 O2 156.9(5) . . ?
O13 V3 O6 80.0(5) . . ?
O13 V3 O8 86.6(6) . . ?
O5 V4 O6 77.1(5) . . ?
O9 V4 O5 86.4(6) . . ?
O9 V4 O6 77.8(5) . . ?
O14 V4 O5 105.1(7) . . ?
O14 V4 O6 177.6(8) . . ?
O14 V4 O9 103.2(8) . . ?
O14 V4 O15 100.0(7) . . ?
O14 V4 O16 99.6(9) . . ?
O15 V4 O5 154.9(5) . . ?
O15 V4 O6 77.8(5) . . ?
O15 V4 O9 88.3(6) . . ?
O16 V4 O5 84.9(7) . . ?
O16 V4 O6 79.5(5) . . ?
O16 V4 O9 157.0(5) . . ?
O16 V4 O15 90.6(7) . . ?
O4 V5 O6 75.7(5) . . ?
O4 V5 O12 84.6(5) . . ?
O4 V5 O16 88.0(6) . . ?
O12 V5 O6 73.7(5) . . ?
O16 V5 O6 77.9(6) . . ?
O16 V5 O12 151.6(7) . . ?
O18 V5 O4 152.4(7) . . ?
O18 V5 O6 77.0(7) . . ?
O18 V5 O12 83.8(6) . . ?
O18 V5 O16 90.6(7) . . ?
O19 V5 O4 103.7(8) . . ?
O19 V5 O6 175.6(9) . . ?
O19 V5 O12 101.9(9) . . ?
O19 V5 O16 106.5(10) . . ?
O19 V5 O18 103.2(9) . . ?
O10 V6 O6 76.5(5) . . ?
O10 V6 O15 86.7(6) . . ?
O13 V6 O6 75.6(5) . . ?
O13 V6 O10 84.5(6) . . ?
O13 V6 O15 152.0(5) . . ?
O13 V6 O18 86.4(7) . . ?
O15 V6 O6 76.5(5) . . ?
O17 V6 O6 178.6(7) . . ?
O17 V6 O10 102.3(7) . . ?
O17 V6 O13 103.7(6) . . ?
O17 V6 O15 104.1(7) . . ?
O17 V6 O18 104.2(8) . . ?
O18 V6 O6 77.0(5) . . ?
O18 V6 O10 153.4(6) . . ?
O18 V6 O15 89.8(6) . . ?
C2 O2 Mo1 117.9(11) . . ?
C2 O2 Mo3 119.1(9) . . ?
C2 O2 V1 117.9(11) . . ?
C2 O2 V3 119.1(9) . . ?
C1 O3 Mo1 114.5(12) . . ?
C1 O3 Mo2 117.4(10) . . ?
C1 O3 V1 114.5(12) . . ?
C1 O3 V2 117.4(10) . . ?
C3 O8 Mo2 119.5(11) . . ?
C3 O8 Mo3 118.6(10) . . ?
C3 O8 V2 119.5(11) . . ?
C3 O8 V3 118.6(10) . . ?
C6 O77 C5 117.8(15) . . ?
O3 C1 H1A 108.5 . . ?
O3 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
C4 C1 O3 115.1(18) . . ?
C4 C1 H1A 108.5 . . ?
C4 C1 H1B 108.5 . . ?
O2 C2 H2A 109.0 . . ?
O2 C2 H2B 109.0 . . ?
O2 C2 C4 113.0(15) . . ?
H2A C2 H2B 107.8 . . ?
C4 C2 H2A 109.0 . . ?
C4 C2 H2B 109.0 . . ?
O8 C3 H3A 109.2 . . ?
O8 C3 H3B 109.2 . . ?
O8 C3 C4 112.3(14) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C1 C4 C2 105.3(17) . . ?
C1 C4 C3 118.4(18) . . ?
C1 C4 C5 107.9(18) . . ?
C3 C4 C2 112.2(16) . . ?
C5 C4 C2 106.6(17) . . ?
C5 C4 C3 105.8(15) . . ?
O77 C5 C4 112.6(16) . . ?
O77 C5 H5A 109.1 . . ?
O77 C5 H5B 109.1 . . ?
C4 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
O78 C6 O77 124(2) . . ?
O78 C6 C7 126(3) . . ?
C7 C6 O77 109(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O20 Mo7 O21 96.9(5) . . ?
O20 Mo7 O22 106.5(6) . . ?
O20 Mo7 O23 105.5(6) . . ?
O20 Mo7 O24 94.9(5) . . ?
O20 Mo7 O25 168.5(5) . . ?
O21 Mo7 O25 76.0(5) . . ?
O22 Mo7 O21 85.1(5) . . ?
O22 Mo7 O24 155.0(5) . . ?
O22 Mo7 O25 82.2(5) . . ?
O23 Mo7 O21 156.5(6) . . ?
O23 Mo7 O22 95.2(6) . . ?
O23 Mo7 O24 91.4(5) . . ?
O23 Mo7 O25 80.7(6) . . ?
O24 Mo7 O21 79.4(5) . . ?
O24 Mo7 O25 75.0(4) . . ?
O21 Mo8 O25 75.4(5) . . ?
O21 Mo8 O27 82.1(5) . . ?
O26 Mo8 O21 97.3(6) . . ?
O26 Mo8 O25 168.8(5) . . ?
O26 Mo8 O27 95.5(5) . . ?
O26 Mo8 O28 104.7(6) . . ?
O26 Mo8 O29 104.0(6) . . ?
O27 Mo8 O25 75.3(4) . . ?
O28 Mo8 O21 90.2(6) . . ?
O28 Mo8 O25 84.0(5) . . ?
O28 Mo8 O27 159.1(5) . . ?
O29 Mo8 O21 156.3(5) . . ?
O29 Mo8 O25 81.9(5) . . ?
O29 Mo8 O27 85.7(6) . . ?
O29 Mo8 O28 94.2(7) . . ?
O24 Mo9 O25 75.8(5) . . ?
O27 Mo9 O24 80.9(5) . . ?
O27 Mo9 O25 78.6(4) . . ?
O30 Mo9 O24 97.5(6) . . ?
O30 Mo9 O25 171.6(6) . . ?
O30 Mo9 O27 95.5(6) . . ?
O30 Mo9 O31 105.0(6) . . ?
O30 Mo9 O32 103.3(7) . . ?
O31 Mo9 O24 89.5(5) . . ?
O31 Mo9 O25 80.2(5) . . ?
O31 Mo9 O27 158.4(5) . . ?
O31 Mo9 O32 93.4(6) . . ?
O32 Mo9 O24 157.5(5) . . ?
O32 Mo9 O25 82.6(5) . . ?
O32 Mo9 O27 88.4(5) . . ?
O29 Mo10 O25 76.9(5) . . ?
O29 Mo10 O32 85.2(6) . . ?
O32 Mo10 O25 74.7(5) . . ?
O33 Mo10 O25 177.0(6) . . ?
O33 Mo10 O29 105.1(6) . . ?
O33 Mo10 O32 103.2(6) . . ?
O33 Mo10 O34 101.2(7) . . ?
O33 Mo10 O35 101.8(7) . . ?
O34 Mo10 O25 76.7(5) . . ?
O34 Mo10 O29 153.5(5) . . ?
O34 Mo10 O32 86.0(6) . . ?
O35 Mo10 O25 80.2(5) . . ?
O35 Mo10 O29 89.9(6) . . ?
O35 Mo10 O32 154.9(6) . . ?
O35 Mo10 O34 87.6(6) . . ?
O23 Mo11 O25 74.6(5) . . ?
O31 Mo11 O23 88.1(5) . . ?
O31 Mo11 O25 75.5(5) . . ?
O31 Mo11 O34 89.1(6) . . ?
O31 Mo11 O36 154.2(5) . . ?
O34 Mo11 O23 153.4(5) . . ?
O34 Mo11 O25 79.1(5) . . ?
O34 Mo11 O36 86.9(6) . . ?
O36 Mo11 O23 84.2(6) . . ?
O36 Mo11 O25 78.7(5) . . ?
O37 Mo11 O23 103.9(7) . . ?
O37 Mo11 O25 178.5(6) . . ?
O37 Mo11 O31 104.6(7) . . ?
O37 Mo11 O34 102.4(6) . . ?
O37 Mo11 O36 101.2(7) . . ?
O22 Mo12 O25 77.3(5) . . ?
O22 Mo12 O28 87.0(6) . . ?
O22 Mo12 O35 155.8(5) . . ?
O28 Mo12 O25 78.4(5) . . ?
O28 Mo12 O35 85.2(6) . . ?
O35 Mo12 O25 78.7(5) . . ?
O36 Mo12 O22 91.0(6) . . ?
O36 Mo12 O25 77.4(5) . . ?
O36 Mo12 O28 155.6(5) . . ?
O36 Mo12 O35 86.7(6) . . ?
O38 Mo12 O22 100.0(7) . . ?
O38 Mo12 O25 177.4(7) . . ?
O38 Mo12 O28 101.7(7) . . ?
O38 Mo12 O35 104.0(7) . . ?
O38 Mo12 O36 102.6(7) . . ?
O20 V7 O21 96.9(5) . . ?
O20 V7 O22 106.5(6) . . ?
O20 V7 O23 105.5(6) . . ?
O20 V7 O24 94.9(5) . . ?
O20 V7 O25 168.5(5) . . ?
O21 V7 O25 76.0(5) . . ?
O22 V7 O21 85.1(5) . . ?
O22 V7 O24 155.0(5) . . ?
O22 V7 O25 82.2(5) . . ?
O23 V7 O21 156.5(6) . . ?
O23 V7 O22 95.2(6) . . ?
O23 V7 O24 91.4(5) . . ?
O23 V7 O25 80.7(6) . . ?
O24 V7 O21 79.4(5) . . ?
O24 V7 O25 75.0(4) . . ?
O21 V8 O25 75.4(5) . . ?
O21 V8 O27 82.1(5) . . ?
O26 V8 O21 97.3(6) . . ?
O26 V8 O25 168.8(5) . . ?
O26 V8 O27 95.5(5) . . ?
O26 V8 O28 104.7(6) . . ?
O26 V8 O29 104.0(6) . . ?
O27 V8 O25 75.3(4) . . ?
O28 V8 O21 90.2(6) . . ?
O28 V8 O25 84.0(5) . . ?
O28 V8 O27 159.1(5) . . ?
O29 V8 O21 156.3(5) . . ?
O29 V8 O25 81.9(5) . . ?
O29 V8 O27 85.7(6) . . ?
O29 V8 O28 94.2(7) . . ?
O24 V9 O25 75.8(5) . . ?
O27 V9 O24 80.9(5) . . ?
O27 V9 O25 78.6(4) . . ?
O30 V9 O24 97.5(6) . . ?
O30 V9 O25 171.6(6) . . ?
O30 V9 O27 95.5(6) . . ?
O30 V9 O31 105.0(6) . . ?
O30 V9 O32 103.3(7) . . ?
O31 V9 O24 89.5(5) . . ?
O31 V9 O25 80.2(5) . . ?
O31 V9 O27 158.4(5) . . ?
O31 V9 O32 93.4(6) . . ?
O32 V9 O24 157.5(5) . . ?
O32 V9 O25 82.6(5) . . ?
O32 V9 O27 88.4(5) . . ?
O29 V10 O25 76.9(5) . . ?
O29 V10 O32 85.2(6) . . ?
O32 V10 O25 74.7(5) . . ?
O33 V10 O25 177.0(6) . . ?
O33 V10 O29 105.1(6) . . ?
O33 V10 O32 103.2(6) . . ?
O33 V10 O34 101.2(7) . . ?
O33 V10 O35 101.8(7) . . ?
O34 V10 O25 76.7(5) . . ?
O34 V10 O29 153.5(5) . . ?
O34 V10 O32 86.0(6) . . ?
O35 V10 O25 80.2(5) . . ?
O35 V10 O29 89.9(6) . . ?
O35 V10 O32 154.9(6) . . ?
O35 V10 O34 87.6(6) . . ?
O23 V11 O25 74.6(5) . . ?
O31 V11 O23 88.1(5) . . ?
O31 V11 O25 75.5(5) . . ?
O31 V11 O34 89.1(6) . . ?
O31 V11 O36 154.2(5) . . ?
O34 V11 O23 153.4(5) . . ?
O34 V11 O25 79.1(5) . . ?
O34 V11 O36 86.9(6) . . ?
O36 V11 O23 84.2(6) . . ?
O36 V11 O25 78.7(5) . . ?
O37 V11 O23 103.9(7) . . ?
O37 V11 O25 178.5(6) . . ?
O37 V11 O31 104.6(7) . . ?
O37 V11 O34 102.4(6) . . ?
O37 V11 O36 101.2(7) . . ?
O22 V12 O25 77.3(5) . . ?
O22 V12 O28 87.0(6) . . ?
O22 V12 O35 155.8(5) . . ?
O28 V12 O25 78.4(5) . . ?
O28 V12 O35 85.2(6) . . ?
O35 V12 O25 78.7(5) . . ?
O36 V12 O22 91.0(6) . . ?
O36 V12 O25 77.4(5) . . ?
O36 V12 O28 155.6(5) . . ?
O36 V12 O35 86.7(6) . . ?
O38 V12 O22 100.0(7) . . ?
O38 V12 O25 177.4(7) . . ?
O38 V12 O28 101.7(7) . . ?
O38 V12 O35 104.0(7) . . ?
O38 V12 O36 102.6(7) . . ?
C9 O21 Mo7 117.7(10) . . ?
C9 O21 Mo8 119.6(10) . . ?
C9 O21 V7 117.7(10) . . ?
C9 O21 V8 119.6(10) . . ?
C8 O24 Mo7 121.9(10) . . ?
C8 O24 Mo9 119.7(11) . . ?
C8 O24 V7 121.9(10) . . ?
C8 O24 V9 119.7(11) . . ?
C10 O27 Mo8 117.4(9) . . ?
C10 O27 Mo9 118.0(10) . . ?
C10 O27 V8 117.4(9) . . ?
C10 O27 V9 118.0(10) . . ?
C13 O79 C12 113.1(18) . . ?
O24 C8 H8A 109.7 . . ?
O24 C8 H8B 109.7 . . ?
O24 C8 C11 110.0(14) . . ?
H8A C8 H8B 108.2 . . ?
C11 C8 H8A 109.7 . . ?
C11 C8 H8B 109.7 . . ?
O21 C9 H9A 109.9 . . ?
O21 C9 H9B 109.9 . . ?
O21 C9 C11 109.0(13) . . ?
H9A C9 H9B 108.3 . . ?
C11 C9 H9A 109.9 . . ?
C11 C9 H9B 109.9 . . ?
O27 C10 H10A 108.2 . . ?
O27 C10 H10B 108.2 . . ?
O27 C10 C11 116.5(15) . . ?
H10A C10 H10B 107.3 . . ?
C11 C10 H10A 108.2 . . ?
C11 C10 H10B 108.2 . . ?
C8 C11 C12 109.4(15) . . ?
C9 C11 C8 110.7(15) . . ?
C9 C11 C12 104.6(13) . . ?
C10 C11 C8 108.9(14) . . ?
C10 C11 C9 113.1(15) . . ?
C10 C11 C12 110.2(16) . . ?
O79 C12 C11 111.9(15) . . ?
O79 C12 H12A 109.2 . . ?
O79 C12 H12B 109.2 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
O80 C13 O79 127(2) . . ?
O80 C13 C14 123(3) . . ?
C14 C13 O79 108(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O39 Mo13 O40 112.3(7) . . ?
O39 Mo13 O41 98.4(7) . . ?
O39 Mo13 O42 95.7(7) . . ?
O39 Mo13 O43 114.2(7) . . ?
O39 Mo13 O44 166.6(7) . . ?
O40 Mo13 O41 80.2(7) . . ?
O40 Mo13 O42 147.5(7) . . ?
O40 Mo13 O43 122.8(7) . . ?
O40 Mo13 O44 78.2(6) . . ?
O41 Mo13 O43 122.7(6) . . ?
O41 Mo13 O44 74.7(6) . . ?
O42 Mo13 O41 79.6(6) . . ?
O42 Mo13 O43 52.5(6) . . ?
O42 Mo13 O44 72.0(6) . . ?
O43 Mo13 O44 62.8(6) . . ?
O42 Mo14 O43 46.0(5) . . ?
O44 Mo14 O42 71.2(6) . . ?
O44 Mo14 O43 58.7(5) . . ?
O45 Mo14 O42 94.3(11) . . ?
O45 Mo14 O43 116.4(11) . . ?
O45 Mo14 O44 163.7(12) . . ?
O45 Mo14 O46 96.7(12) . . ?
O45 Mo14 O56 116.5(13) . . ?
O45 Mo14 O57 108.9(11) . . ?
O46 Mo14 O42 73.2(8) . . ?
O46 Mo14 O43 109.5(7) . . ?
O46 Mo14 O44 72.5(8) . . ?
O56 Mo14 O42 148.4(9) . . ?
O56 Mo14 O43 108.7(9) . . ?
O56 Mo14 O44 79.0(9) . . ?
O56 Mo14 O46 107.9(11) . . ?
O56 Mo14 O57 74.2(9) . . ?
O57 Mo14 O42 89.8(6) . . ?
O57 Mo14 O43 45.7(5) . . ?
O57 Mo14 O44 79.2(6) . . ?
O57 Mo14 O46 150.4(8) . . ?
O41 Mo15 O44 75.5(6) . . ?
O46 Mo15 O41 80.4(8) . . ?
O46 Mo15 O44 75.6(8) . . ?
O46 Mo15 O48 155.1(10) . . ?
O47 Mo15 O41 94.5(8) . . ?
O47 Mo15 O44 169.3(8) . . ?
O47 Mo15 O46 99.1(9) . . ?
O47 Mo15 O48 101.6(10) . . ?
O48 Mo15 O41 84.3(8) . . ?
O48 Mo15 O44 81.7(8) . . ?
O49 Mo15 O41 141.4(8) . . ?
O49 Mo15 O44 68.8(7) . . ?
O49 Mo15 O46 104.0(10) . . ?
O49 Mo15 O47 121.8(9) . . ?
O49 Mo15 O48 76.5(9) . . ?
O49 Mo16 O44 63.2(7) . . ?
O49 Mo16 O51 71.5(8) . . ?
O49 Mo16 O54 137.1(10) . . ?
O49 Mo16 O55 120.6(9) . . ?
O49 Mo16 O56 106.3(9) . . ?
O51 Mo16 O44 82.0(6) . . ?
O51 Mo16 O54 99.3(9) . . ?
O51 Mo16 O56 147.4(9) . . ?
O54 Mo16 O44 74.1(9) . . ?
O55 Mo16 O44 175.3(9) . . ?
O55 Mo16 O51 101.8(8) . . ?
O55 Mo16 O54 102.2(10) . . ?
O55 Mo16 O56 106.5(10) . . ?
O56 Mo16 O44 69.1(8) . . ?
O56 Mo16 O54 59.3(11) . . ?
O40 Mo17 O44 70.2(6) . . ?
O40 Mo17 O51 148.2(7) . . ?
O40 Mo17 O52 88.9(6) . . ?
O48 Mo17 O40 81.7(9) . . ?
O48 Mo17 O44 75.1(8) . . ?
O48 Mo17 O51 85.0(9) . . ?
O48 Mo17 O52 152.7(9) . . ?
O50 Mo17 O40 99.9(7) . . ?
O50 Mo17 O44 170.0(7) . . ?
O50 Mo17 O48 102.7(9) . . ?
O50 Mo17 O51 111.1(7) . . ?
O50 Mo17 O52 104.1(6) . . ?
O51 Mo17 O44 78.5(6) . . ?
O51 Mo17 O52 90.0(6) . . ?
O52 Mo17 O44 77.5(5) . . ?
O43 Mo18 O44 63.2(6) . . ?
O52 Mo18 O43 123.1(6) . . ?
O52 Mo18 O44 87.2(6) . . ?
O52 Mo18 O57 158.6(6) . . ?
O53 Mo18 O43 112.0(6) . . ?
O53 Mo18 O44 171.6(6) . . ?
O53 Mo18 O52 101.2(6) . . ?
O53 Mo18 O54 94.0(10) . . ?
O53 Mo18 O57 99.9(6) . . ?
O54 Mo18 O43 118.7(10) . . ?
O54 Mo18 O44 83.1(10) . . ?
O54 Mo18 O52 103.0(10) . . ?
O54 Mo18 O57 71.4(9) . . ?
O57 Mo18 O43 50.6(5) . . ?
O57 Mo18 O44 71.7(5) . . ?
O39 V13 O40 112.3(7) . . ?
O39 V13 O41 98.4(7) . . ?
O39 V13 O42 95.7(7) . . ?
O39 V13 O43 114.2(7) . . ?
O39 V13 O44 166.6(7) . . ?
O40 V13 O41 80.2(7) . . ?
O40 V13 O42 147.5(7) . . ?
O40 V13 O43 122.8(7) . . ?
O40 V13 O44 78.2(6) . . ?
O41 V13 O43 122.7(6) . . ?
O41 V13 O44 74.7(6) . . ?
O42 V13 O41 79.6(6) . . ?
O42 V13 O43 52.5(6) . . ?
O42 V13 O44 72.0(6) . . ?
O43 V13 O44 62.8(6) . . ?
O42 V14 O43 46.0(5) . . ?
O44 V14 O42 71.2(6) . . ?
O44 V14 O43 58.7(5) . . ?
O45 V14 O42 94.3(11) . . ?
O45 V14 O43 116.4(11) . . ?
O45 V14 O44 163.7(12) . . ?
O45 V14 O46 96.7(12) . . ?
O45 V14 O56 116.5(13) . . ?
O45 V14 O57 108.9(11) . . ?
O46 V14 O42 73.2(8) . . ?
O46 V14 O43 109.5(7) . . ?
O46 V14 O44 72.5(8) . . ?
O56 V14 O42 148.4(9) . . ?
O56 V14 O43 108.7(9) . . ?
O56 V14 O44 79.0(9) . . ?
O56 V14 O46 107.9(11) . . ?
O56 V14 O57 74.2(9) . . ?
O57 V14 O42 89.8(6) . . ?
O57 V14 O43 45.7(5) . . ?
O57 V14 O44 79.2(6) . . ?
O57 V14 O46 150.4(8) . . ?
O41 V15 O44 75.5(6) . . ?
O46 V15 O41 80.4(8) . . ?
O46 V15 O44 75.6(8) . . ?
O46 V15 O48 155.1(10) . . ?
O47 V15 O41 94.5(8) . . ?
O47 V15 O44 169.3(8) . . ?
O47 V15 O46 99.1(9) . . ?
O47 V15 O48 101.6(10) . . ?
O48 V15 O41 84.3(8) . . ?
O48 V15 O44 81.7(8) . . ?
O49 V15 O41 141.4(8) . . ?
O49 V15 O44 68.8(7) . . ?
O49 V15 O46 104.0(10) . . ?
O49 V15 O47 121.8(9) . . ?
O49 V15 O48 76.5(9) . . ?
O49 V16 O44 63.2(7) . . ?
O49 V16 O51 71.5(8) . . ?
O49 V16 O54 137.1(10) . . ?
O49 V16 O55 120.6(9) . . ?
O49 V16 O56 106.3(9) . . ?
O51 V16 O44 82.0(6) . . ?
O51 V16 O54 99.3(9) . . ?
O51 V16 O56 147.4(9) . . ?
O54 V16 O44 74.1(9) . . ?
O55 V16 O44 175.3(9) . . ?
O55 V16 O51 101.8(8) . . ?
O55 V16 O54 102.2(10) . . ?
O55 V16 O56 106.5(10) . . ?
O56 V16 O44 69.1(8) . . ?
O56 V16 O54 59.3(11) . . ?
O40 V17 O51 148.2(7) . . ?
O40 V17 O52 88.9(6) . . ?
O48 V17 O40 81.7(9) . . ?
O48 V17 O51 85.0(9) . . ?
O48 V17 O52 152.7(9) . . ?
O50 V17 O40 99.9(7) . . ?
O50 V17 O48 102.7(9) . . ?
O50 V17 O51 111.1(7) . . ?
O50 V17 O52 104.1(6) . . ?
O51 V17 O52 90.0(6) . . ?
O43 V18 O44 63.2(6) . . ?
O52 V18 O43 123.1(6) . . ?
O52 V18 O44 87.2(6) . . ?
O52 V18 O57 158.6(6) . . ?
O53 V18 O43 112.0(6) . . ?
O53 V18 O44 171.6(6) . . ?
O53 V18 O52 101.2(6) . . ?
O53 V18 O54 94.0(10) . . ?
O53 V18 O57 99.9(6) . . ?
O54 V18 O43 118.7(10) . . ?
O54 V18 O44 83.1(10) . . ?
O54 V18 O52 103.0(10) . . ?
O54 V18 O57 71.4(9) . . ?
O57 V18 O43 50.6(5) . . ?
O57 V18 O44 71.7(5) . . ?
C15 O41 Mo13 117.3(14) . . ?
C15 O41 Mo15 122.0(14) . . ?
C15 O41 V13 117.3(14) . . ?
C15 O41 V15 122.0(14) . . ?
O43 O42 Mo13 65.0(6) . . ?
O43 O42 Mo14 74.3(7) . . ?
O43 O42 V13 65.0(6) . . ?
O43 O42 V14 74.3(7) . . ?
C16 O42 Mo13 122.2(13) . . ?
C16 O42 Mo14 117.6(14) . . ?
C16 O42 V13 122.2(13) . . ?
C16 O42 V14 117.6(14) . . ?
C16 O42 O43 155.6(15) . . ?
O42 O43 Mo13 62.5(6) . . ?
O42 O43 Mo14 59.7(7) . . ?
O42 O43 Mo18 138.8(9) . . ?
O42 O43 V13 62.5(6) . . ?
O42 O43 V14 59.7(7) . . ?
O42 O43 V18 138.8(9) . . ?
O57 O43 Mo13 139.3(9) . . ?
O57 O43 Mo14 46.4(5) . . ?
O57 O43 Mo18 64.3(5) . . ?
O57 O43 V13 139.3(9) . . ?
O57 O43 V14 46.4(5) . . ?
O57 O43 V18 64.3(5) . . ?
O57 O43 O42 103.8(10) . . ?
C17 O46 Mo14 122.8(16) . . ?
C17 O46 Mo15 121.6(17) . . ?
C17 O46 V14 122.8(16) . . ?
C17 O46 V15 121.6(17) . . ?
O43 O57 Mo14 87.9(7) . . ?
O43 O57 Mo18 65.1(6) . . ?
O43 O57 V14 87.9(7) . . ?
O43 O57 V18 65.1(6) . . ?
C20 O81 C19 110.6(19) . . ?
O41 C15 H15A 110.0 . . ?
O41 C15 H15B 110.0 . . ?
O41 C15 C18 108.5(16) . . ?
H15A C15 H15B 108.4 . . ?
C18 C15 H15A 110.0 . . ?
C18 C15 H15B 110.0 . . ?
O42 C16 H16A 108.3 . . ?
O42 C16 H16B 108.3 . . ?
O42 C16 C18 116.0(19) . . ?
H16A C16 H16B 107.4 . . ?
C18 C16 H16A 108.3 . . ?
C18 C16 H16B 108.3 . . ?
O46 C17 H17A 108.0 . . ?
O46 C17 H17B 108.0 . . ?
H17A C17 H17B 107.3 . . ?
C18 C17 O46 117(2) . . ?
C18 C17 H17A 108.0 . . ?
C18 C17 H17B 108.0 . . ?
C16 C18 C15 97.5(16) . . ?
C16 C18 C19 113.1(18) . . ?
C17 C18 C15 102.6(18) . . ?
C17 C18 C16 112(2) . . ?
C17 C18 C19 121(2) . . ?
C19 C18 C15 106.8(15) . . ?
O81 C19 C18 102.2(17) . . ?
O81 C19 H19A 111.3 . . ?
O81 C19 H19B 111.3 . . ?
C18 C19 H19A 111.3 . . ?
C18 C19 H19B 111.3 . . ?
H19A C19 H19B 109.2 . . ?
O81 C20 O82 126(2) . . ?
O81 C20 C21 120(2) . . ?
O82 C20 C21 114(2) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O58 Mo19 O59 106.9(11) . . ?
O58 Mo19 O60 101.6(11) . . ?
O58 Mo19 O61 105.0(12) . . ?
O58 Mo19 O62 115.2(11) . . ?
O58 Mo19 O63 170.3(11) . . ?
O59 Mo19 O60 78.5(8) . . ?
O59 Mo19 O61 146.3(9) . . ?
O59 Mo19 O62 97.6(8) . . ?
O59 Mo19 O63 78.2(7) . . ?
O60 Mo19 O63 71.0(7) . . ?
O61 Mo19 O60 84.9(9) . . ?
O61 Mo19 O62 78.0(9) . . ?
O61 Mo19 O63 68.7(8) . . ?
O62 Mo19 O60 142.2(8) . . ?
O62 Mo19 O63 71.5(8) . . ?
O60 Mo20 O63 74.4(8) . . ?
O60 Mo20 O65 85.0(8) . . ?
O60 Mo20 O66 154.3(9) . . ?
O60 Mo20 O67 91.1(9) . . ?
O64 Mo20 O60 98.0(11) . . ?
O64 Mo20 O63 172.1(10) . . ?
O64 Mo20 O65 102.3(10) . . ?
O64 Mo20 O66 107.4(10) . . ?
O64 Mo20 O67 103.7(10) . . ?
O65 Mo20 O63 75.6(7) . . ?
O65 Mo20 O67 154.0(8) . . ?
O66 Mo20 O63 80.2(8) . . ?
O66 Mo20 O65 85.5(8) . . ?
O66 Mo20 O67 87.0(9) . . ?
O67 Mo20 O63 78.5(8) . . ?
O61 Mo21 O63 69.3(9) . . ?
O61 Mo21 O65 85.2(9) . . ?
O65 Mo21 O63 75.3(7) . . ?
O68 Mo21 O61 104.9(11) . . ?
O68 Mo21 O63 168.7(10) . . ?
O68 Mo21 O65 94.8(10) . . ?
O68 Mo21 O69 99.8(11) . . ?
O68 Mo21 O70 108.8(11) . . ?
O69 Mo21 O61 153.2(11) . . ?
O69 Mo21 O63 84.5(9) . . ?
O69 Mo21 O65 82.6(9) . . ?
O69 Mo21 O70 104.2(11) . . ?
O70 Mo21 O61 77.6(10) . . ?
O70 Mo21 O63 79.9(9) . . ?
O70 Mo21 O65 153.6(9) . . ?
O66 Mo22 O63 76.4(7) . . ?
O66 Mo22 O69 81.2(9) . . ?
O66 Mo22 O72 152.0(10) . . ?
O69 Mo22 O63 75.3(8) . . ?
O71 Mo22 O63 171.2(12) . . ?
O71 Mo22 O66 95.4(12) . . ?
O71 Mo22 O69 100.5(13) . . ?
O71 Mo22 O72 112.6(14) . . ?
O71 Mo22 O73 105.9(14) . . ?
O72 Mo22 O63 75.7(9) . . ?
O72 Mo22 O69 92.8(10) . . ?
O73 Mo22 O63 76.6(9) . . ?
O73 Mo22 O66 83.3(10) . . ?
O73 Mo22 O69 150.4(11) . . ?
O73 Mo22 O72 89.2(11) . . ?
O62 Mo23 O63 74.6(9) . . ?
O62 Mo23 O70 79.0(10) . . ?
O62 Mo23 O72 153.3(11) . . ?
O62 Mo23 O74 101.4(12) . . ?
O62 Mo23 O75 89.1(9) . . ?
O70 Mo23 O63 74.9(8) . . ?
O72 Mo23 O63 78.8(9) . . ?
O72 Mo23 O70 92.3(11) . . ?
O74 Mo23 O63 174.3(11) . . ?
O74 Mo23 O70 100.5(12) . . ?
O74 Mo23 O72 105.0(13) . . ?
O74 Mo23 O75 109.4(11) . . ?
O75 Mo23 O63 74.9(6) . . ?
O75 Mo23 O70 149.5(9) . . ?
O75 Mo23 O72 85.8(9) . . ?
O59 Mo24 O63 74.6(7) . . ?
O59 Mo24 O73 148.5(10) . . ?
O59 Mo24 O75 90.8(7) . . ?
O67 Mo24 O59 85.8(9) . . ?
O67 Mo24 O63 82.3(9) . . ?
O67 Mo24 O73 78.6(10) . . ?
O67 Mo24 O75 153.6(9) . . ?
O73 Mo24 O63 76.3(9) . . ?
O75 Mo24 O63 71.6(6) . . ?
O75 Mo24 O73 91.3(9) . . ?
O76 Mo24 O59 105.0(10) . . ?
O76 Mo24 O63 178.7(10) . . ?
O76 Mo24 O67 98.9(11) . . ?
O76 Mo24 O73 104.4(11) . . ?
O76 Mo24 O75 107.2(9) . . ?
O58 V19 O59 106.9(11) . . ?
O58 V19 O60 101.6(11) . . ?
O58 V19 O61 105.0(12) . . ?
O58 V19 O62 115.2(11) . . ?
O58 V19 O63 170.3(11) . . ?
O59 V19 O60 78.5(8) . . ?
O59 V19 O61 146.3(9) . . ?
O59 V19 O62 97.6(8) . . ?
O59 V19 O63 78.2(7) . . ?
O60 V19 O63 71.0(7) . . ?
O61 V19 O60 84.9(9) . . ?
O61 V19 O62 78.0(9) . . ?
O61 V19 O63 68.7(8) . . ?
O62 V19 O60 142.2(8) . . ?
O62 V19 O63 71.5(8) . . ?
O60 V20 O63 74.4(8) . . ?
O60 V20 O65 85.0(8) . . ?
O60 V20 O66 154.3(9) . . ?
O60 V20 O67 91.1(9) . . ?
O64 V20 O60 98.0(11) . . ?
O64 V20 O63 172.1(10) . . ?
O64 V20 O65 102.3(10) . . ?
O64 V20 O66 107.4(10) . . ?
O64 V20 O67 103.7(10) . . ?
O65 V20 O63 75.6(7) . . ?
O65 V20 O67 154.0(8) . . ?
O66 V20 O63 80.2(8) . . ?
O66 V20 O65 85.5(8) . . ?
O66 V20 O67 87.0(9) . . ?
O67 V20 O63 78.5(8) . . ?
O61 V21 O63 69.3(9) . . ?
O61 V21 O65 85.2(9) . . ?
O65 V21 O63 75.3(7) . . ?
O68 V21 O61 104.9(11) . . ?
O68 V21 O63 168.7(10) . . ?
O68 V21 O65 94.8(10) . . ?
O68 V21 O69 99.8(11) . . ?
O68 V21 O70 108.8(11) . . ?
O69 V21 O61 153.2(11) . . ?
O69 V21 O63 84.5(9) . . ?
O69 V21 O65 82.6(9) . . ?
O69 V21 O70 104.2(11) . . ?
O70 V21 O61 77.6(10) . . ?
O70 V21 O63 79.9(9) . . ?
O70 V21 O65 153.6(9) . . ?
O66 V22 O63 76.4(7) . . ?
O66 V22 O69 81.2(9) . . ?
O66 V22 O72 152.0(10) . . ?
O69 V22 O63 75.3(8) . . ?
O71 V22 O63 171.2(12) . . ?
O71 V22 O66 95.4(12) . . ?
O71 V22 O69 100.5(13) . . ?
O71 V22 O72 112.6(14) . . ?
O71 V22 O73 105.9(14) . . ?
O72 V22 O63 75.7(9) . . ?
O72 V22 O69 92.8(10) . . ?
O73 V22 O63 76.6(9) . . ?
O73 V22 O66 83.3(10) . . ?
O73 V22 O69 150.4(11) . . ?
O73 V22 O72 89.2(11) . . ?
O62 V23 O63 74.6(9) . . ?
O62 V23 O70 79.0(10) . . ?
O62 V23 O72 153.3(11) . . ?
O62 V23 O74 101.4(12) . . ?
O62 V23 O75 89.1(9) . . ?
O70 V23 O63 74.9(8) . . ?
O72 V23 O63 78.8(9) . . ?
O72 V23 O70 92.3(11) . . ?
O74 V23 O63 174.3(11) . . ?
O74 V23 O70 100.5(12) . . ?
O74 V23 O72 105.0(13) . . ?
O74 V23 O75 109.4(11) . . ?
O75 V23 O63 74.9(6) . . ?
O75 V23 O70 149.5(9) . . ?
O75 V23 O72 85.8(9) . . ?
O59 V24 O63 74.6(7) . . ?
O59 V24 O73 148.5(10) . . ?
O59 V24 O75 90.8(7) . . ?
O67 V24 O59 85.8(9) . . ?
O67 V24 O63 82.3(9) . . ?
O67 V24 O73 78.6(10) . . ?
O67 V24 O75 153.6(9) . . ?
O73 V24 O63 76.3(9) . . ?
O75 V24 O63 71.6(6) . . ?
O75 V24 O73 91.3(9) . . ?
O76 V24 O59 105.0(10) . . ?
O76 V24 O63 178.7(10) . . ?
O76 V24 O67 98.9(11) . . ?
O76 V24 O73 104.4(11) . . ?
O76 V24 O75 107.2(9) . . ?
C23 O60 Mo19 113.7(15) . . ?
C23 O60 Mo20 121.0(17) . . ?
C23 O60 V19 113.7(15) . . ?
C23 O60 V20 121.0(17) . . ?
C22 O61 Mo19 101.9(16) . . ?
C22 O61 Mo21 118.2(18) . . ?
C22 O61 V19 101.9(16) . . ?
C22 O61 V21 118.2(18) . . ?
C24 O65 Mo20 117.7(14) . . ?
C24 O65 Mo21 121.2(14) . . ?
C24 O65 V20 117.7(14) . . ?
C24 O65 V21 121.2(14) . . ?
C27 O83 C26 110.9(13) . . ?
O61 C22 H22A 107.3 . . ?
O61 C22 H22B 107.3 . . ?
H22A C22 H22B 106.9 . . ?
C25 C22 O61 119.9(19) . . ?
C25 C22 H22A 107.3 . . ?
C25 C22 H22B 107.3 . . ?
O60 C23 H23A 110.6 . . ?
O60 C23 H23B 110.6 . . ?
O60 C23 C25 105.5(18) . . ?
H23A C23 H23B 108.8 . . ?
C25 C23 H23A 110.6 . . ?
C25 C23 H23B 110.6 . . ?
O65 C24 H24A 111.5 . . ?
O65 C24 H24B 111.5 . . ?
O65 C24 C25 101.6(17) . . ?
H24A C24 H24B 109.3 . . ?
C25 C24 H24A 111.5 . . ?
C25 C24 H24B 111.5 . . ?
C22 C25 C23 108.2(18) . . ?
C22 C25 C24 114.4(19) . . ?
C22 C25 C26 114.6(18) . . ?
C23 C25 C26 108.4(17) . . ?
C24 C25 C23 105.2(17) . . ?
C24 C25 C26 105.5(17) . . ?
O83 C26 C25 99.9(15) . . ?
O83 C26 H26A 111.8 . . ?
O83 C26 H26B 111.8 . . ?
C25 C26 H26A 111.8 . . ?
C25 C26 H26B 111.8 . . ?
H26A C26 H26B 109.5 . . ?
O84 C27 O83 120.5(15) . . ?
O84 C27 C28 139(2) . . ?
C28 C27 O83 99.0(14) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 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 -0.864 -0.956 -0.691 8277.0 912.8 'N2 C32 H72'
_shelx_fab_file
;
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18 -6 10 -0.6300 -0.3578
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18 -5 1 -2.3714 -0.2489
18 -5 2 -0.5529 1.0104
18 -5 3 6.6779 -0.0123
18 -5 4 -7.8370 0.0094
18 -5 5 -2.9865 0.3430
18 -5 6 2.0301 -0.3610
18 -5 7 7.1800 -0.4958
18 -5 8 11.7749 0.6608
18 -5 9 -3.5958 -0.7858
18 -5 10 -7.4549 0.7167
18 -5 11 -4.1305 -0.2019
18 -4 0 -5.0797 -0.2243
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18 -4 2 -0.8964 -0.1830
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18 -4 10 -2.9619 -0.4709
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18 -3 1 -6.7907 0.7911
18 -3 2 11.1763 -0.7900
18 -3 3 -11.4189 -0.1168
18 -3 4 3.7145 0.3844
18 -3 5 22.8518 -0.6507
18 -3 6 -7.0709 1.2551
18 -3 7 -1.3936 0.0561
18 -3 8 -4.2400 -0.3392
18 -3 9 12.4948 0.9083
18 -3 10 -8.8471 -1.2894
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18 -2 0 0.2975 1.9405
18 -2 1 3.2856 -1.2540
18 -2 2 -3.2164 -1.0912
18 -2 3 4.3969 1.1384
18 -2 4 -4.4153 0.0206
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18 -1 7 3.0728 0.5059
18 -1 8 0.8085 0.0920
18 -1 9 2.6068 0.0033
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18 2 8 0.3366 0.3314
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18 3 2 -2.2163 0.2846
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18 3 5 10.4513 -0.4457
18 3 6 -3.8885 0.3749
18 3 7 1.7196 0.0782
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18 3 9 5.2252 -0.2570
18 3 10 -0.4354 1.6600
18 3 11 -5.6467 -1.7823
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18 4 5 -9.7502 -0.2067
18 4 6 -5.4194 0.2129
18 4 7 0.0502 0.1843
18 4 8 0.5538 0.1122
18 4 9 -6.3482 0.4927
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18 6 7 12.2500 0.1159
18 6 8 2.0067 0.5706
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18 7 2 -0.7669 -0.9928
18 7 3 1.5929 0.3552
18 7 4 10.2587 -0.2334
18 7 5 5.6682 0.3643
18 7 6 -6.5313 0.7085
18 7 7 -3.7490 0.1353
18 7 8 9.1072 0.3160
18 8 0 2.1555 0.1841
18 8 1 3.8329 -0.7199
18 8 2 -2.9283 -0.1337
18 8 3 -0.4394 0.2895
18 8 4 2.6303 0.1487
18 8 5 -3.9141 0.0451
18 8 6 -15.5744 -0.4772
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18 10 3 -6.4288 0.2471
18 10 4 -2.1964 -0.4630
18 10 5 4.1830 0.7249
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18 11 2 -3.0935 -0.5630
18 11 3 2.3297 1.2512
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19 -2 9 -1.7949 -1.0292
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19 -1 1 1.9811 2.5270
19 -1 2 -1.6010 1.0044
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19 0 8 -3.3687 0.0683
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19 1 3 -12.1697 0.6443
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19 1 5 0.3292 0.1205
19 1 6 -8.3684 0.4322
19 1 7 -2.4153 -0.1471
19 1 8 -1.8666 -0.4428
19 1 9 -0.7390 0.0230
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19 2 9 2.7308 0.2110
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19 3 4 -0.6235 -0.1997
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19 6 7 -6.3329 -0.0290
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19 7 1 5.6161 1.0015
19 7 2 5.7553 0.3235
19 7 3 7.3269 -0.5453
19 7 4 -7.6639 -0.2641
19 7 5 11.3357 0.4811
19 7 6 -0.7031 -0.7140
19 8 0 2.8749 0.6653
19 8 1 -2.9953 -1.3818
19 8 2 5.8419 -0.2225
19 8 3 0.5159 0.9207
19 8 4 -2.7890 -0.5273
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19 9 3 7.6009 -0.3269
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20 -8 1 7.8060 -0.5998
20 -8 2 -12.5480 0.7372
20 -7 0 -1.2603 0.0346
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20 -7 2 1.4360 0.2133
20 -7 3 -4.5648 -0.5906
20 -7 4 -5.9587 0.2888
20 -6 0 -7.5688 1.0081
20 -6 1 1.1238 -1.0037
20 -6 2 -0.6201 -0.0791
20 -6 3 -4.1395 0.7192
20 -6 4 -2.6330 -0.3661
20 -6 5 1.5061 0.3393
20 -5 0 -3.9352 1.8029
20 -5 1 -6.9787 -1.6475
20 -5 2 -1.8933 0.4850
20 -5 3 8.1557 0.0679
20 -5 4 -12.0949 0.2132
20 -5 5 1.4261 0.3722
20 -5 6 6.7475 0.1817
20 -4 0 5.6291 -2.0724
20 -4 1 4.3879 2.0319
20 -4 2 -5.5708 0.5420
20 -4 3 -3.5672 -0.5436
20 -4 4 1.3301 0.2874
20 -4 5 -0.0693 -1.3879
20 -4 6 2.7233 0.9331
20 -3 0 10.9794 -2.4413
20 -3 1 -5.0798 2.2095
20 -3 2 -4.5461 0.3725
20 -3 3 -1.9660 -1.1140
20 -3 4 6.0754 0.0686
20 -3 5 4.9830 -0.2847
20 -3 6 1.0849 0.9617
20 -3 7 -4.2255 -0.6089
20 -2 0 8.2259 -0.5718
20 -2 1 0.6616 0.0511
20 -2 2 -17.3142 0.0259
20 -2 3 2.9935 0.2328
20 -2 4 -0.5562 -0.1256
20 -2 5 -4.6017 0.8261
20 -2 6 -3.1290 -0.9810
20 -2 7 -0.2928 1.6284
20 -1 0 -4.0423 2.0530
20 -1 1 -0.8632 -1.5745
20 -1 2 -2.3185 -0.3100
20 -1 3 2.4367 0.6101
20 -1 4 -4.3066 -0.3723
20 -1 5 0.3042 0.2405
20 -1 6 9.2803 -1.1384
20 -1 7 6.6461 1.0797
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20 0 2 -2.9231 -0.7980
20 0 3 -2.8781 0.0071
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20 0 5 3.9716 0.0162
20 0 6 -5.1596 0.2552
20 0 7 8.3736 0.3629
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20 1 1 -3.0963 -0.8910
20 1 2 -0.3670 -1.0538
20 1 3 -3.0028 1.1896
20 1 4 -2.9757 -0.1918
20 1 5 -5.2513 0.7235
20 1 6 13.0758 -0.0022
20 1 7 -1.0943 -0.0676
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20 2 1 1.4993 0.5266
20 2 2 -3.3963 0.4493
20 2 3 -7.0437 -0.7147
20 2 4 6.6734 0.3322
20 2 5 11.3742 -0.8600
20 2 6 1.3600 0.3961
20 3 0 6.1132 -0.3861
20 3 1 5.6662 0.0166
20 3 2 -6.6531 1.3390
20 3 3 -1.3169 -1.1206
20 3 4 -4.3531 0.6962
20 3 5 -5.7713 -1.1979
20 3 6 11.0576 0.7508
20 4 0 6.3554 -0.5568
20 4 1 0.8543 0.6026
20 4 2 -6.8926 -0.1673
20 4 3 0.8958 0.6286
20 4 4 -7.3069 -0.6321
20 4 5 7.4242 0.6349
20 5 0 -1.3945 -0.1564
20 5 1 6.1817 -0.0607
20 5 2 4.6440 0.1067
20 5 3 -8.7401 0.1732
20 5 4 7.3402 -0.0079
20 6 0 0.2954 -0.7164
20 6 1 -4.1939 0.4601
20 6 2 -7.4794 -0.6225
20 6 3 11.3688 1.2042
20 7 0 2.9581 -0.7944
20 7 1 -1.0124 0.7666
21 -5 0 -4.7074 -0.1005
21 -4 0 4.5254 0.0118
21 -4 1 2.8242 -0.5704
21 -4 2 -5.8010 0.6343
21 -3 0 5.9915 0.1019
21 -3 1 -1.5243 0.7372
21 -3 2 0.7745 -0.4039
21 -2 0 -0.6005 3.1628
21 -2 1 -9.0110 -2.8804
21 -2 2 -6.3756 -0.6895
21 -2 3 8.3800 1.5615
21 -1 0 -3.8030 1.8646
21 -1 1 4.1014 -1.7150
21 -1 2 -1.0170 -0.8488
21 -1 3 -6.7412 1.3954
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21 0 1 -1.7420 1.6511
21 0 2 -4.6516 0.4055
21 0 3 -7.6383 -1.4546
21 1 0 -1.1883 -3.0759
21 1 1 1.3818 2.3077
21 1 2 -8.3284 0.2271
21 1 3 -8.3606 -0.9362
21 2 0 -1.6816 -1.6499
21 2 1 -3.8241 0.8396
21 2 2 -10.0667 0.1410
21 3 0 12.5524 0.9613
21 3 1 -0.1470 -1.0692
0 0 0 0.0 0.0
;
_iucr_refine_instructions_details
;
hk-6-42.res created by SHELXL-2014/7
TITL hk-6-42_a.res in P-1
REM Old TITL HK-6-42 in P-1
REM SHELXT solution in P-1
REM R1 0.290, Rweak 0.016, Alpha 0.084, Orientation as input
REM Formula found by SHELXT: V3 Mo3 O21 N2 C39 H83
CELL 1.54184 21.4889 22.7196 24.1556 90.952 93.807 91.862
ZERR 8 0.0013 0.0017 0.0017 0.006 0.005 0.005
LATT 1
SFAC V Mo O N C H
UNIT 24 24 168 16 312 664
DFIX 1.22 C27 O84
DFIX 1.45 C27 C28
DFIX 1.45 0.01 C28 C27
DFIX 2 Mo13 O43
DFIX 2 Mo18 O43
DFIX 1.4 C15 O41
DFIX 2 Mo18 O52
DFIX 2 O52 Mo17
DANG 2.3 O84 O83
DANG 2.35 O83 C28
DANG 2.35 O84 C28
FLAT O83 O84 C27 C28
EADP V2 Mo2
EADP Mo2 V2
EADP V1 Mo1
EADP V3 Mo3
EADP Mo6 V6
EADP Mo4 V4
EADP Mo5 V5
EADP V5 Mo5
EADP V6 Mo6
EADP V4 Mo4
EADP Mo8 V8
EADP Mo9 V9
EADP V8 Mo8
EADP Mo7 V7
EADP Mo11 V11
EADP Mo12 V12
EADP Mo10 V10
EADP Mo23 V23
EADP Mo19 V19
EADP Mo20 V20
EADP V20 Mo20
EADP Mo22 V22
EADP Mo24 V24
EADP V23 Mo23
EADP V19 Mo19
EADP Mo21 V21
EADP Mo17 V17
EADP Mo18 V18
EADP Mo13 V13
EADP Mo14 V14
EADP Mo15 V15
EADP Mo16 V16
EADP V14 Mo14
EADP V18 Mo18
EADP V17 Mo17
EADP V13 Mo13
EADP V15 Mo15
EADP V16 Mo16
EXYZ Mo2 V2
EXYZ V1 Mo1
EXYZ V3 Mo3
EXYZ V5 Mo5
EXYZ V6 Mo6
EXYZ V4 Mo4
EXYZ Mo9 V9
EXYZ V8 Mo8
EXYZ Mo7 V7
EXYZ Mo11 V11
EXYZ Mo12 V12
EXYZ Mo10 V10
EXYZ V20 Mo20
EXYZ Mo22 V22
EXYZ Mo24 V24
EXYZ V23 Mo23
EXYZ V19 Mo19
EXYZ Mo21 V21
EXYZ V14 Mo14
EXYZ V18 Mo18
EXYZ V17 Mo17
EXYZ V13 Mo13
EXYZ V15 Mo15
EXYZ V16 Mo16
L.S. 30
PLAN 80
BOND $H
list 4
ABIN
fmap 2 53
acta
REM
REM
REM
WGHT 0.200000
FVAR 0.47777
PART 6
MO1 2 0.104217 0.678588 0.555203 10.25000 0.09717 0.09102 =
0.08281 -0.02092 0.01795 -0.02099
PART 0
PART 3
MO2 2 0.164523 0.744876 0.446494 10.50000 0.11225 0.11308 =
0.07574 -0.01407 0.01281 -0.00893
PART 0
PART 8
MO3 2 0.250682 0.730499 0.565704 10.25000 0.08314 0.09182 =
0.06531 -0.01619 0.00894 -0.01040
PART 0
PART 14
MO4 2 0.134204 0.609153 0.446585 10.75000 0.12035 0.11517 =
0.09073 -0.03525 0.01180 -0.02612
PART 0
PART 10
MO5 2 0.216717 0.594834 0.560494 10.50000 0.10689 0.07497 =
0.06948 -0.00460 0.01427 -0.00025
PART 0
PART 12
MO6 2 0.277403 0.659241 0.456972 10.75000 0.10093 0.09858 =
0.07856 -0.02053 0.02934 -0.00363
PART 0
PART 5
V1 1 0.104217 0.678588 0.555203 10.75000 0.09717 0.09102 =
0.08281 -0.02092 0.01795 -0.02099
PART 0
PART 4
V2 1 0.164523 0.744876 0.446494 10.50000 0.11225 0.11308 =
0.07574 -0.01407 0.01281 -0.00893
PART 0
PART 7
V3 1 0.250682 0.730499 0.565704 10.75000 0.08314 0.09182 =
0.06531 -0.01619 0.00894 -0.01040
PART 0
PART 13
V4 1 0.134204 0.609153 0.446585 10.25000 0.12035 0.11517 =
0.09073 -0.03525 0.01180 -0.02612
PART 0
PART 9
V5 1 0.216717 0.594834 0.560494 10.50000 0.10689 0.07497 =
0.06948 -0.00460 0.01427 -0.00025
PART 0
PART 11
V6 1 0.277403 0.659241 0.456972 10.25000 0.10093 0.09858 =
0.07856 -0.02053 0.02934 -0.00363
PART 0
O1 3 0.046080 0.693097 0.585765 11.00000 0.08222 0.09859 =
0.15236 -0.03505 0.02225 -0.01716
O2 3 0.163335 0.736694 0.597877 11.00000 0.09409 0.08500 =
0.06430 -0.02944 0.02667 -0.03065
O3 3 0.093732 0.745050 0.502244 11.00000 0.09092 0.08202 =
0.08038 0.00552 0.01311 0.00097
O4 3 0.142849 0.623765 0.591239 11.00000 0.10049 0.08205 =
0.06796 -0.01662 0.01554 -0.01944
O5 3 0.072756 0.630839 0.500111 11.00000 0.09668 0.12894 =
0.08544 -0.04138 0.03179 -0.04785
O6 3 0.191271 0.676065 0.506897 11.00000 0.08417 0.06875 =
0.10008 -0.00338 -0.00108 0.00547
O7 3 0.142951 0.801948 0.410944 11.00000 0.13464 0.08626 =
0.06798 -0.00182 0.01320 0.00855
O8 3 0.213237 0.791392 0.510121 11.00000 0.08437 0.09571 =
0.05545 -0.00197 0.00829 -0.00728
O9 3 0.117595 0.683441 0.412259 11.00000 0.11968 0.09101 =
0.05304 -0.00965 0.00460 -0.01410
O10 3 0.240591 0.726904 0.421364 11.00000 0.10500 0.09658 =
0.05324 -0.00133 0.01212 0.02101
O11 3 0.286503 0.781109 0.608142 11.00000 0.07699 0.09064 =
0.09680 -0.02699 0.00872 -0.00830
O12 3 0.258328 0.662639 0.598182 11.00000 0.09701 0.08290 =
0.09769 -0.02779 -0.00035 0.01262
O13 3 0.307055 0.714685 0.513224 11.00000 0.07786 0.11790 =
0.09370 -0.04389 0.04181 -0.01716
O14 3 0.095640 0.559377 0.402144 11.00000 0.15742 0.19087 =
0.08013 -0.08657 0.00683 -0.06794
O15 3 0.210840 0.611773 0.417226 11.00000 0.10098 0.10826 =
0.06608 -0.02139 0.01546 -0.01007
O16 3 0.163174 0.559337 0.500524 11.00000 0.12172 0.09497 =
0.10507 -0.05564 0.02617 -0.02948
O17 3 0.338734 0.648914 0.421039 11.00000 0.10336 0.10914 =
0.12904 -0.03019 0.05407 -0.01576
O18 3 0.283400 0.601112 0.513442 11.00000 0.11029 0.12303 =
0.14228 -0.05945 0.05070 -0.00920
O19 3 0.234055 0.549620 0.595301 11.00000 0.09500 0.34177 =
0.09802 -0.08528 0.04455 -0.02149
O77 3 0.052727 0.885254 0.608333 11.00000 0.08555 0.08931 =
0.09016 -0.01897 0.02762 -0.01433
O78 3 0.067195 0.977618 0.646586 11.00000 0.12807 0.11050 =
0.14013 -0.04145 0.03770 -0.02562
C1 5 0.079553 0.804960 0.529851 11.00000 0.08058 0.12081 =
0.09975 -0.00193 0.03296 0.00285
AFIX 23
H1A 6 0.064896 0.831395 0.501053 11.00000 -1.20000
H1B 6 0.045896 0.798614 0.554153 11.00000 -1.20000
AFIX 0
C2 5 0.140293 0.795029 0.610808 11.00000 0.06132 0.08790 =
0.09994 -0.04853 0.01914 -0.00679
AFIX 23
H2A 6 0.170319 0.815478 0.636710 11.00000 -1.20000
H2B 6 0.101484 0.790267 0.628841 11.00000 -1.20000
AFIX 0
C3 5 0.187445 0.844567 0.532204 11.00000 0.10669 0.06681 =
0.04496 -0.00190 0.00746 -0.00473
AFIX 23
H3A 6 0.178839 0.871528 0.502146 11.00000 -1.20000
H3B 6 0.218098 0.863656 0.558454 11.00000 -1.20000
AFIX 0
C4 5 0.129370 0.832210 0.560174 11.00000 0.08133 0.07884 =
0.07657 -0.00018 -0.00831 -0.01156
C5 5 0.109134 0.889884 0.580052 11.00000 0.10098 0.07336 =
0.09008 0.00329 0.00898 0.00404
AFIX 23
H5A 6 0.141933 0.907728 0.604988 11.00000 -1.20000
H5B 6 0.102769 0.915569 0.548645 11.00000 -1.20000
AFIX 0
C6 5 0.038036 0.933293 0.642467 11.00000 0.08738 0.16075 =
0.07760 -0.00007 0.03531 -0.00208
C7 5 -0.018229 0.923149 0.661900 11.00000 0.20034 0.15186 =
0.06314 -0.01451 -0.00541 -0.04049
AFIX 137
H7A 6 -0.038196 0.889393 0.643004 11.00000 -1.50000
H7B 6 -0.043332 0.956898 0.655652 11.00000 -1.50000
H7C 6 -0.013461 0.915890 0.700966 11.00000 -1.50000
AFIX 0
PART 19
MO7 2 0.277278 0.060148 0.538678 10.50000 0.09627 0.09934 =
0.08246 -0.00935 0.00885 0.00203
PART 0
PART 18
MO8 2 0.234784 0.196082 0.572843 10.25000 0.08139 0.09586 =
0.06875 -0.01360 0.00952 -0.00185
PART 0
PART 15
MO9 2 0.225709 0.152144 0.440568 10.25000 0.08857 0.10644 =
0.05754 -0.00876 0.00850 0.00586
PART 0
PART 25
MO10 2 0.325796 0.249271 0.487810 10.75000 0.09179 0.08426 =
0.07996 -0.00763 0.02033 -0.00354
PART 0
PART 21
MO11 2 0.365562 0.118236 0.452528 10.75000 0.08159 0.10383 =
0.07135 -0.01521 0.01804 0.00798
PART 0
PART 23
MO12 2 0.375381 0.158840 0.583064 10.50000 0.06377 0.09682 =
0.05322 -0.01147 0.00072 -0.00451
PART 0
PART 20
V7 1 0.277278 0.060148 0.538678 10.50000 0.09627 0.09934 =
0.08246 -0.00935 0.00885 0.00203
PART 0
PART 17
V8 1 0.234784 0.196082 0.572843 10.75000 0.08139 0.09586 =
0.06875 -0.01360 0.00952 -0.00185
PART 0
PART 16
V9 1 0.225709 0.152144 0.440568 10.75000 0.08857 0.10644 =
0.05754 -0.00876 0.00850 0.00586
PART 0
PART 26
V10 1 0.325796 0.249271 0.487810 10.25000 0.09179 0.08426 =
0.07996 -0.00763 0.02033 -0.00354
PART 0
PART 22
V11 1 0.365562 0.118236 0.452528 10.25000 0.08159 0.10383 =
0.07135 -0.01521 0.01804 0.00798
PART 0
PART 24
V12 1 0.375381 0.158840 0.583064 10.50000 0.06377 0.09682 =
0.05322 -0.01147 0.00072 -0.00451
PART 0
O20 3 0.250331 -0.004801 0.555467 11.00000 0.07183 0.10003 =
0.07538 -0.00604 0.01078 0.01578
O21 3 0.217916 0.108248 0.581917 11.00000 0.08956 0.08109 =
0.05268 -0.00351 0.01334 0.00422
O22 3 0.336967 0.083489 0.594493 11.00000 0.08463 0.09519 =
0.07353 0.00988 0.00028 0.00419
O23 3 0.331315 0.046776 0.488531 11.00000 0.08477 0.11485 =
0.07428 0.00273 0.01960 0.01663
O24 3 0.208384 0.073133 0.478697 11.00000 0.08906 0.07575 =
0.04145 -0.00968 0.01077 -0.00589
O25 3 0.294063 0.152389 0.510942 11.00000 0.05466 0.11802 =
0.07821 -0.01346 0.01786 -0.01559
O26 3 0.182437 0.218625 0.610987 11.00000 0.08734 0.09607 =
0.07097 -0.01584 0.00865 -0.00495
O27 3 0.175117 0.181594 0.502215 11.00000 0.06504 0.08599 =
0.04359 -0.00877 0.00761 0.01027
O28 3 0.305691 0.192840 0.620035 11.00000 0.06788 0.15206 =
0.06591 -0.02183 0.01280 0.00813
O29 3 0.261386 0.262231 0.538585 11.00000 0.10642 0.08582 =
0.07815 -0.01486 0.04556 0.00100
O30 3 0.168570 0.147437 0.394626 11.00000 0.10136 0.12071 =
0.05378 -0.01313 0.01313 0.01723
O31 3 0.290369 0.119698 0.407813 11.00000 0.05853 0.08541 =
0.08173 -0.00748 0.00568 0.00822
O32 3 0.256406 0.227123 0.433630 11.00000 0.07677 0.11022 =
0.05932 0.00363 0.00020 0.00091
O33 3 0.347592 0.315181 0.468445 11.00000 0.11128 0.15535 =
0.06723 -0.01361 0.01143 0.01260
O34 3 0.375790 0.200490 0.443934 11.00000 0.09028 0.09864 =
0.08032 -0.02237 0.03751 0.00044
O35 3 0.384064 0.236595 0.549049 11.00000 0.07511 0.09827 =
0.09018 -0.00595 -0.00718 0.00559
O36 3 0.416761 0.128491 0.521942 11.00000 0.07254 0.11070 =
0.07315 -0.01397 -0.00611 0.00522
O37 3 0.418206 0.091078 0.409879 11.00000 0.08353 0.12189 =
0.13230 -0.02472 0.05747 0.01419
O38 3 0.432951 0.160222 0.635772 11.00000 0.08865 0.15814 =
0.08199 -0.01721 -0.03075 -0.01420
O79 3 0.024413 0.095842 0.577857 11.00000 0.08807 0.10874 =
0.05607 -0.02360 0.03088 0.00941
O80 3 -0.056613 0.036304 0.565938 11.00000 0.11411 0.17678 =
0.18085 -0.12028 0.06665 -0.07395
C8 5 0.149011 0.054154 0.483967 11.00000 0.08272 0.10105 =
0.03687 -0.02402 -0.00787 0.01593
AFIX 23
H8A 6 0.148350 0.013265 0.494911 11.00000 -1.20000
H8B 6 0.125196 0.056714 0.448594 11.00000 -1.20000
AFIX 0
C9 5 0.153128 0.085369 0.583981 11.00000 0.04970 0.09192 =
0.06387 -0.00567 0.01983 -0.01580
AFIX 23
H9A 6 0.132182 0.107171 0.611734 11.00000 -1.20000
H9B 6 0.152960 0.044227 0.594097 11.00000 -1.20000
AFIX 0
C10 5 0.118191 0.154113 0.508874 11.00000 0.05248 0.16616 =
0.03538 -0.02590 -0.01734 0.01255
AFIX 23
H10A 6 0.093594 0.154950 0.473759 11.00000 -1.20000
H10B 6 0.096771 0.176983 0.535551 11.00000 -1.20000
AFIX 0
C11 5 0.119350 0.091772 0.527672 11.00000 0.09089 0.08092 =
0.04247 0.00473 0.01062 -0.00046
C12 5 0.051142 0.067479 0.535084 11.00000 0.10423 0.09131 =
0.08231 -0.01063 -0.03480 -0.00025
AFIX 23
H12A 6 0.025749 0.072540 0.500882 11.00000 -1.20000
H12B 6 0.052105 0.025659 0.542409 11.00000 -1.20000
AFIX 0
C13 5 -0.026615 0.070249 0.591211 11.00000 0.08682 0.21220 =
0.07311 -0.03463 0.04496 0.04399
C14 5 -0.043729 0.095919 0.629410 11.00000 0.12074 0.17302 =
0.33741 0.13220 -0.08376 -0.10119
AFIX 137
H14A 6 -0.083060 0.112991 0.619286 11.00000 -1.50000
H14B 6 -0.013594 0.126558 0.640924 11.00000 -1.50000
H14C 6 -0.048578 0.069277 0.659375 11.00000 -1.50000
AFIX 0
PART 46
MO13 2 0.342134 0.215666 -0.056462 10.50000 0.19691 0.25982 =
0.10898 -0.03309 0.02033 0.03031
PART 0
PART 40
MO14 2 0.376067 0.142187 0.063670 10.50000 0.30616 0.26991 =
0.14006 -0.05307 -0.04762 0.10127
PART 0
PART 48
MO15 2 0.264039 0.232638 0.056583 10.50000 0.27386 0.35904 =
0.15697 -0.08129 0.04146 0.00855
PART 0
PART 50
MO16 2 0.236471 0.100773 0.062395 10.50000 0.54483 0.30390 =
0.07340 -0.04910 0.08248 -0.19159
PART 0
PART 44
MO17 2 0.199423 0.169681 -0.050566 10.50000 0.23019 0.19091 =
0.07412 -0.02616 0.01177 0.05278
PART 0
PART 42
MO18 2 0.312137 0.082771 -0.045572 10.50000 0.31129 0.14884 =
0.07407 -0.01108 0.00178 0.02846
PART 0
PART 45
V13 1 0.342134 0.215666 -0.056462 10.50000 0.19691 0.25982 =
0.10898 -0.03309 0.02033 0.03031
PART 0
PART 39
V14 1 0.376067 0.142187 0.063670 10.50000 0.30616 0.26991 =
0.14006 -0.05307 -0.04762 0.10127
PART 0
PART 47
V15 1 0.264039 0.232638 0.056583 10.50000 0.27386 0.35904 =
0.15697 -0.08129 0.04146 0.00855
PART 0
PART 49
V16 1 0.236471 0.100773 0.062395 10.50000 0.54483 0.30390 =
0.07340 -0.04910 0.08248 -0.19159
PART 0
PART 43
V17 1 0.199423 0.169681 -0.050566 10.50000 0.23019 0.19091 =
0.07412 -0.02616 0.01177 0.05278
PART 0
PART 41
V18 1 0.312137 0.082771 -0.045572 10.50000 0.31129 0.14884 =
0.07407 -0.01108 0.00178 0.02846
PART 0
O39 3 0.386334 0.262395 -0.092780 11.00000 10.10000
O40 3 0.260818 0.217410 -0.078354 11.00000 10.10000
O41 3 0.314110 0.273860 -0.000640 11.00000 10.10000
O42 3 0.406428 0.205275 0.005525 11.00000 10.10000
O43 3 0.384811 0.140186 -0.034248 11.00000 10.10000
O44 3 0.299146 0.161651 0.007763 11.00000 0.11102
O45 3 0.440245 0.146162 0.101615 11.00000 0.18749
O46 3 0.343742 0.222198 0.087640 11.00000 0.14755
O47 3 0.247587 0.296850 0.091056 11.00000 10.10000
O48 3 0.199265 0.228576 -0.001161 11.00000 0.16402
O49 3 0.227309 0.170632 0.067174 11.00000 10.10000
O50 3 0.137669 0.184809 -0.096243 11.00000 10.10000
O51 3 0.173254 0.121604 0.008250 11.00000 10.10000
O52 3 0.237438 0.100710 -0.084540 11.00000 10.10000
O53 3 0.330752 0.021886 -0.078961 11.00000 10.07000
O54 3 0.285861 0.043240 0.014226 11.00000 0.20022
O55 3 0.196951 0.053799 0.101999 11.00000 10.10000
O56 3 0.322818 0.089021 0.079763 11.00000 0.14995
O57 3 0.380404 0.086757 0.014346 11.00000 10.07000
O81 3 0.428790 0.392130 0.107527 11.00000 10.10000
O82 3 0.518126 0.423302 0.148119 11.00000 10.10000
C15 5 0.353492 0.321880 0.013051 11.00000 10.10000
AFIX 23
H15A 6 0.330395 0.353038 0.029296 11.00000 -1.20000
H15B 6 0.371404 0.336812 -0.019973 11.00000 -1.20000
AFIX 0
C16 5 0.446573 0.251527 0.025905 11.00000 10.10000
AFIX 23
H16A 6 0.462442 0.271953 -0.005447 11.00000 -1.20000
H16B 6 0.481902 0.234823 0.046416 11.00000 -1.20000
AFIX 0
C17 5 0.384311 0.271170 0.104803 11.00000 10.10000
AFIX 23
H17A 6 0.359480 0.300755 0.121443 11.00000 -1.20000
H17B 6 0.414009 0.258014 0.133602 11.00000 -1.20000
AFIX 0
C18 5 0.417457 0.297945 0.064418 11.00000 10.10000
C19 5 0.464931 0.357600 0.079172 11.00000 10.10000
AFIX 23
H19A 6 0.502020 0.347328 0.101549 11.00000 -1.20000
H19B 6 0.477221 0.376328 0.045603 11.00000 -1.20000
AFIX 0
C20 5 0.459953 0.425678 0.137418 11.00000 10.10000
C21 5 0.431474 0.467715 0.169334 11.00000 10.10000
AFIX 137
H21A 6 0.402622 0.489080 0.145935 11.00000 -1.50000
H21B 6 0.462757 0.494557 0.186378 11.00000 -1.50000
H21C 6 0.409499 0.448353 0.197589 11.00000 -1.50000
AFIX 0
PART 36
MO19 2 0.268321 0.598635 0.074347 10.50000 0.24429 0.28743 =
0.10535 -0.02217 0.00931 0.02677
PART 0
PART 28
MO20 2 0.212352 0.570228 -0.055470 10.50000 0.20647 0.20066 =
0.09051 -0.02548 0.01702 -0.04672
PART 0
PART 37
MO21 2 0.306190 0.687533 -0.027115 10.50000 0.17913 0.20171 =
0.12340 -0.00195 0.02368 -0.03292
PART 0
PART 29
MO22 2 0.164643 0.701395 -0.060470 10.50000 0.14979 0.16781 =
0.09016 -0.00752 0.00433 0.01759
PART 0
PART 34
MO23 2 0.219302 0.727804 0.066227 10.50000 0.17219 0.17100 =
0.10529 -0.03542 0.01059 0.00338
PART 0
PART 31
MO24 2 0.124298 0.616349 0.037641 10.50000 0.14619 0.19460 =
0.11655 -0.02559 0.03126 -0.02296
PART 0
PART 35
V19 1 0.268321 0.598635 0.074347 10.50000 0.24429 0.28743 =
0.10535 -0.02217 0.00931 0.02677
PART 0
PART 27
V20 1 0.212352 0.570228 -0.055470 10.50000 0.20647 0.20066 =
0.09051 -0.02548 0.01702 -0.04672
PART 0
PART 38
V21 1 0.306190 0.687533 -0.027115 10.50000 0.17913 0.20171 =
0.12340 -0.00195 0.02368 -0.03292
PART 0
PART 30
V22 1 0.164643 0.701395 -0.060470 10.50000 0.14979 0.16781 =
0.09016 -0.00752 0.00433 0.01759
PART 0
PART 33
V23 1 0.219302 0.727804 0.066227 10.50000 0.17219 0.17100 =
0.10529 -0.03542 0.01059 0.00338
PART 0
PART 32
V24 1 0.124298 0.616349 0.037641 10.50000 0.14619 0.19460 =
0.11655 -0.02559 0.03126 -0.02296
PART 0
O58 3 0.308537 0.559228 0.115580 11.00000 0.17980
O59 3 0.181477 0.572554 0.078232 11.00000 0.12101
O60 3 0.254954 0.542295 0.003056 11.00000 0.13379
O61 3 0.329292 0.640962 0.031617 11.00000 0.16739
O62 3 0.259342 0.682288 0.099987 11.00000 0.14109
O63 3 0.223118 0.646248 0.007760 11.00000 0.12168
O64 3 0.211896 0.516320 -0.091937 11.00000 0.15077
O65 3 0.290783 0.609757 -0.070720 11.00000 0.12028
O66 3 0.175194 0.628718 -0.096623 11.00000 0.13668
O67 3 0.128919 0.561550 -0.015982 11.00000 0.16593
O68 3 0.375963 0.705918 -0.057281 11.00000 0.18125
O69 3 0.252226 0.713154 -0.078319 11.00000 0.17008
O70 3 0.298464 0.736610 0.032378 11.00000 0.17077
O71 3 0.127660 0.733033 -0.115792 11.00000 0.23997
O72 3 0.175053 0.753258 0.002900 11.00000 0.18826
O73 3 0.104590 0.660089 -0.026432 11.00000 0.18222
O74 3 0.224166 0.785753 0.109589 11.00000 0.21349
O75 3 0.151877 0.684909 0.077525 11.00000 0.08919
O76 3 0.053089 0.595464 0.060729 11.00000 0.17855
O83 3 0.392630 0.459527 -0.078931 11.00000 10.10000
O84 3 0.426460 0.397618 -0.149811 11.00000 10.10000
C22 5 0.377410 0.593265 0.022685 11.00000 10.10000
AFIX 23
H22A 6 0.416398 0.613380 0.015247 11.00000 -1.20000
H22B 6 0.384522 0.573277 0.057597 11.00000 -1.20000
AFIX 0
C23 5 0.303830 0.504241 -0.003240 11.00000 10.10000
AFIX 23
H23A 6 0.292447 0.474782 -0.031974 11.00000 -1.20000
H23B 6 0.314390 0.484436 0.031221 11.00000 -1.20000
AFIX 0
C24 5 0.341752 0.573525 -0.083985 11.00000 10.10000
AFIX 23
H24A 6 0.375042 0.596589 -0.099325 11.00000 -1.20000
H24B 6 0.327968 0.541938 -0.109887 11.00000 -1.20000
AFIX 0
C25 5 0.364342 0.547324 -0.021197 11.00000 10.10000
C26 5 0.425014 0.503917 -0.032080 11.00000 10.10000
AFIX 23
H26A 6 0.459993 0.526141 -0.045647 11.00000 -1.20000
H26B 6 0.438710 0.483348 0.001190 11.00000 -1.20000
AFIX 0
C27 5 0.441711 0.429858 -0.111694 11.00000 10.10000
C28 5 0.495961 0.444696 -0.075740 11.00000 10.10000
AFIX 137
H28A 6 0.507989 0.485293 -0.080339 11.00000 -1.50000
H28B 6 0.529526 0.420225 -0.084912 11.00000 -1.50000
H28C 6 0.486679 0.438500 -0.037903 11.00000 -1.50000
AFIX 0
HKLF 4
REM hk-6-42_a.res in P-1
REM R1 = 0.1501 for 12691 Fo > 4sig(Fo) and 0.1909 for all 24359 data
REM 918 parameters refined using 12 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 3.417, deepest hole -1.934, 1-sigma level 0.198
Q1 1 0.2451 0.0617 -0.0471 11.00000 0.05 2.22
Q2 1 0.2715 0.0397 0.0809 11.00000 0.05 1.97
Q3 1 0.1442 0.1404 -0.0443 11.00000 0.05 1.72
Q4 1 0.3617 0.1380 -0.0791 11.00000 0.05 1.60
Q5 1 0.1436 0.0969 0.0651 11.00000 0.05 1.46
Q6 1 0.1807 0.1573 0.0596 11.00000 0.05 1.41
Q7 1 0.2108 0.5504 0.0854 11.00000 0.05 1.32
Q8 1 0.2422 0.5386 0.6103 11.00000 0.05 1.26
Q9 1 0.3402 0.0564 0.0170 11.00000 0.05 1.12
Q10 1 0.2414 0.7040 0.0807 11.00000 0.05 1.09
Q11 1 0.0988 0.5802 -0.0063 11.00000 0.05 1.07
Q12 1 0.2631 -0.0025 0.5725 11.00000 0.05 1.03
Q13 1 0.2519 0.1759 0.0641 11.00000 0.05 0.99
Q14 1 0.0395 0.6871 0.5968 11.00000 0.05 0.98
Q15 1 0.2185 0.1856 0.0972 11.00000 0.05 0.97
Q16 1 0.2863 0.6585 0.1189 11.00000 0.05 0.96
Q17 1 0.1879 0.6925 0.0773 11.00000 0.05 0.93
Q18 1 0.3295 0.3149 0.4583 11.00000 0.05 0.92
Q19 1 0.1983 0.0853 0.0211 11.00000 0.05 0.89
Q20 1 -0.0465 0.1170 0.6448 11.00000 0.05 0.86
Q21 1 0.2972 0.1170 0.1034 11.00000 0.05 0.85
Q22 1 0.2976 0.6747 0.0263 11.00000 0.05 0.82
Q23 1 0.2959 0.1826 0.6251 11.00000 0.05 0.82
Q24 1 0.2520 0.1392 -0.0821 11.00000 0.05 0.78
Q25 1 0.1429 0.6151 0.6025 11.00000 0.05 0.76
Q26 1 0.3512 0.6234 -0.0788 11.00000 0.05 0.75
Q27 1 0.3361 0.5796 0.0841 11.00000 0.05 0.71
Q28 1 0.4404 0.3487 -0.0873 11.00000 0.05 0.70
Q29 1 0.3464 0.6204 0.0360 11.00000 0.05 0.70
Q30 1 0.3077 0.2825 -0.0640 11.00000 0.05 0.69
Q31 1 0.1375 0.0449 0.4860 11.00000 0.05 0.67
Q32 1 0.3115 0.2994 -0.0443 11.00000 0.05 0.66
Q33 1 0.2782 0.2630 -0.0834 11.00000 0.05 0.65
Q34 1 0.2748 0.5400 0.0165 11.00000 0.05 0.65
Q35 1 0.3512 0.6564 0.4256 11.00000 0.05 0.64
Q36 1 0.1021 0.1577 0.5008 11.00000 0.05 0.64
Q37 1 0.5000 0.5000 0.0000 10.50000 0.05 0.63
Q38 1 0.2982 0.7694 0.6153 11.00000 0.05 0.63
Q39 1 0.1589 0.5674 0.0633 11.00000 0.05 0.63
Q40 1 -0.0217 0.9034 0.6740 11.00000 0.05 0.62
Q41 1 0.4590 0.4806 -0.1236 11.00000 0.05 0.60
Q42 1 0.2923 0.6151 -0.0253 11.00000 0.05 0.60
Q43 1 0.2259 0.2424 -0.0911 11.00000 0.05 0.59
Q44 1 0.4380 0.1256 0.5324 11.00000 0.05 0.59
Q45 1 0.3239 0.6024 0.1185 11.00000 0.05 0.59
Q46 1 0.3856 0.6987 -0.0437 11.00000 0.05 0.58
Q47 1 0.3595 0.7187 -0.0588 11.00000 0.05 0.58
Q48 1 -0.0922 0.0379 0.5436 11.00000 0.05 0.58
Q49 1 -0.0286 0.0014 0.6008 11.00000 0.05 0.57
Q50 1 0.2721 0.5370 0.1235 11.00000 0.05 0.57
Q51 1 0.2615 0.5496 -0.0516 11.00000 0.05 0.57
Q52 1 0.4220 0.4421 -0.1741 11.00000 0.05 0.56
Q53 1 0.1568 0.5426 -0.0184 11.00000 0.05 0.56
Q54 1 0.4344 0.3513 0.1282 11.00000 0.05 0.56
Q55 1 0.4749 0.4259 0.0394 11.00000 0.05 0.55
Q56 1 0.5082 0.5450 -0.0624 11.00000 0.05 0.54
Q57 1 0.3361 0.6639 -0.1004 11.00000 0.05 0.53
Q58 1 0.2628 0.2228 -0.0420 11.00000 0.05 0.52
Q59 1 0.3479 0.2389 0.0590 11.00000 0.05 0.52
Q60 1 0.3182 0.1976 0.0847 11.00000 0.05 0.52
Q61 1 0.3925 0.0816 0.0985 11.00000 0.05 0.51
Q62 1 0.2361 0.4842 -0.0496 11.00000 0.05 0.50
Q63 1 0.2988 0.6404 -0.0635 11.00000 0.05 0.50
Q64 1 0.2561 0.1440 0.0060 11.00000 0.05 0.49
Q65 1 0.3214 0.4988 0.0414 11.00000 0.05 0.48
Q66 1 0.2194 0.2580 -0.0063 11.00000 0.05 0.47
Q67 1 0.2719 0.2545 -0.0035 11.00000 0.05 0.47
Q68 1 0.0961 0.9597 0.6632 11.00000 0.05 0.47
Q69 1 0.2449 0.5140 -0.0961 11.00000 0.05 0.46
Q70 1 0.0084 0.0989 0.5751 11.00000 0.05 0.46
Q71 1 0.1398 0.7579 -0.1095 11.00000 0.05 0.46
Q72 1 0.1670 0.5457 0.5066 11.00000 0.05 0.46
Q73 1 0.4296 0.1655 0.0139 11.00000 0.05 0.45
Q74 1 0.3568 0.6453 -0.0288 11.00000 0.05 0.45
Q75 1 0.2530 0.5073 -0.0735 11.00000 0.05 0.45
Q76 1 0.4301 0.1632 0.0272 11.00000 0.05 0.45
Q77 1 0.2793 0.7635 0.0211 11.00000 0.05 0.44
Q78 1 0.4452 0.5173 0.0232 11.00000 0.05 0.43
Q79 1 0.2206 0.6188 0.4060 11.00000 0.05 0.43
Q80 1 0.2554 0.2443 -0.0013 11.00000 0.05 0.43
REM The information below was added by Olex2.
REM
REM R1 = 0.1501 for 12691 Fo > 4sig(Fo) and 0.1909 for all 43456 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 3.42, deepest hole -1.93
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.1909
REM R1_gt = 0.1501
REM wR_ref = 0.4348
REM GOOF = 1.281
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 43456
REM Reflections_gt = 12691
REM Parameters = n/a
REM Hole = -1.93
REM Peak = 3.42
REM Flack = n/a
;
_olex2_date_sample_data_collection 2017-02-13
_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 1.688
_oxdiff_exptl_absorpt_empirical_full_min 0.559
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
#######################################################################
#
# 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_hk-5-164-amine
_database_code_depnum_ccdc_archive 'CCDC 1553743'
_audit_update_record
;
2017-06-02 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_audit_creation_date 2017-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C4 H8 Mo3 N O19 V3, C16 H36 N, C16 H35 N, C2 H3 N'
_chemical_formula_sum 'C38 H82 Mo3 N4 O19 V3'
_chemical_formula_weight 1339.71
_chemical_melting_point ?
_chemical_oxdiff_formula V3Mo3C22N3O20
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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 monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 15.7948(3)
_cell_length_b 18.5129(3)
_cell_length_c 18.2430(3)
_cell_angle_alpha 90
_cell_angle_beta 100.088(2)
_cell_angle_gamma 90
_cell_volume 5251.92(16)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 12114
_cell_measurement_temperature 130.00(10)
_cell_measurement_theta_max 75.3090
_cell_measurement_theta_min 4.7020
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 10.605
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.54942
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43i (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.694
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description ?
_exptl_crystal_F_000 2740
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0323
_diffrn_reflns_av_unetI/netI 0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 32619
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.787
_diffrn_reflns_theta_min 3.428
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 130.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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 -48.00 35.00 1.00 5.00 -- -40.81 38.00 120.00 83
2 \w -38.00 74.00 1.00 5.00 -- 40.81 -77.00-120.00 112
3 \w 23.00 95.00 1.00 5.00 -- 40.81-125.00-180.00 72
4 \w 44.00 115.00 1.00 10.00 -- 110.21-111.00 -60.00 71
5 \w 46.00 144.00 1.00 10.00 -- 110.21 -77.00 -60.00 98
6 \w 50.00 175.00 1.00 10.00 -- 110.21 15.00-120.00 125
7 \w 80.00 174.00 1.00 10.00 -- 110.21 61.00 -90.00 94
8 \w 32.00 91.00 1.00 10.00 -- 110.21 -30.00 -60.00 59
9 \w 36.00 91.00 1.00 10.00 -- 110.21 -30.00-120.00 55
10 \w 32.00 115.00 1.00 10.00 -- 110.21-111.00 120.00 83
11 \w 31.00 144.00 1.00 10.00 -- 110.21 -77.00 120.00 113
12 \w -115.00 -13.00 1.00 5.00 -- -40.81 -57.00 -30.00 102
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0669563000
_diffrn_orient_matrix_UB_12 -0.0317670000
_diffrn_orient_matrix_UB_13 -0.0431013000
_diffrn_orient_matrix_UB_21 0.0527903000
_diffrn_orient_matrix_UB_22 -0.0281624000
_diffrn_orient_matrix_UB_23 0.0735246000
_diffrn_orient_matrix_UB_31 -0.0504402000
_diffrn_orient_matrix_UB_32 -0.0715589000
_diffrn_orient_matrix_UB_33 -0.0097783000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 9429
_reflns_number_total 10711
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 68.13
_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 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43i (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 1.410
_refine_diff_density_min -1.696
_refine_diff_density_rms 0.215
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.157
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 622
_refine_ls_number_reflns 10711
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0758
_refine_ls_R_factor_gt 0.0693
_refine_ls_restrained_S_all 1.157
_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^)+(0.0869P)^2^+88.6063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2428
_refine_ls_wR_factor_ref 0.2465
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Shared sites
{V6, Mo6}
{Mo1, V1}
{Mo2, V2}
{V4, Mo4}
{V3, Mo3}
{V5, Mo5}
3. Uiso/Uaniso restraints and constraints
Uanis(Mo3) = Uanis(V3)
Uanis(Mo5) = Uanis(V5)
Uanis(Mo6) = Uanis(V6)
Uanis(Mo4) = Uanis(V4)
Uanis(V6) = Uanis(Mo6)
Uanis(Mo1) = Uanis(V1)
Uanis(Mo2) = Uanis(V2)
Uanis(V4) = Uanis(Mo4)
Uanis(V3) = Uanis(Mo3)
Uanis(V5) = Uanis(Mo5)
4. Others
Fixed Sof: Mo1(0.25) Mo2(0.5) Mo3(0.25) Mo4(0.5) Mo5(0.75) Mo6(0.75) V1(0.75)
V2(0.5) V3(0.75) V4(0.5) V5(0.25) V6(0.25)
5.a Secondary CH2 refined with riding coordinates:
C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B),
C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C22(H22A,H22B),
C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,
H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B),
C35(H35A,H35B)
5.b Idealised Me refined as rotating group:
C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C20(H20A,H20B,
H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C36(H36A,
H36B,H36C), C37(H37A,H37B,H37C)
;
_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 0.25176(6) 0.43019(6) 0.25106(6) 0.0213(2) Uani 0.25 1 d . . P A 5
Mo2 Mo 0.19060(5) 0.56059(5) 0.36124(5) 0.0228(2) Uani 0.5 1 d . . P A 7
Mo3 Mo 0.39245(7) 0.55627(7) 0.32832(7) 0.0295(3) Uani 0.25 1 d . . P A 12
Mo4 Mo 0.26185(6) 0.67530(5) 0.25991(6) 0.0302(2) Uani 0.5 1 d . . P A 10
Mo5 Mo 0.32207(5) 0.55299(5) 0.15563(4) 0.0281(2) Uani 0.75 1 d . . P A 14
Mo6 Mo 0.12449(5) 0.55613(4) 0.18576(4) 0.0241(2) Uani 0.75 1 d . . P A 4
V1 V 0.25176(6) 0.43019(6) 0.25106(6) 0.0213(2) Uani 0.75 1 d . . P A 6
V2 V 0.19060(5) 0.56059(5) 0.36124(5) 0.0228(2) Uani 0.5 1 d . . P A 8
V3 V 0.39245(7) 0.55627(7) 0.32832(7) 0.0295(3) Uani 0.75 1 d . . P A 11
V4 V 0.26185(6) 0.67530(5) 0.25991(6) 0.0302(2) Uani 0.5 1 d . . P A 9
V5 V 0.32207(5) 0.55299(5) 0.15563(4) 0.0281(2) Uani 0.25 1 d . . P A 13
V6 V 0.12449(5) 0.55613(4) 0.18576(4) 0.0241(2) Uani 0.25 1 d . . P A 3
O1 O 0.2526(4) 0.3433(4) 0.2585(4) 0.0355(15) Uani 1 1 d . . . . .
O2 O 0.2067(3) 0.4489(3) 0.3491(3) 0.0226(11) Uani 1 1 d . . . . .
O3 O 0.3675(4) 0.4485(3) 0.3207(3) 0.0246(12) Uani 1 1 d . . . . .
O4 O 0.3057(4) 0.4503(3) 0.1732(3) 0.0291(13) Uani 1 1 d . . . . .
O5 O 0.1436(4) 0.4528(3) 0.2024(3) 0.0272(12) Uani 1 1 d . . . . .
O6 O 0.2585(3) 0.5496(3) 0.2648(3) 0.0216(11) Uani 1 1 d . . . . .
O7 O 0.3195(3) 0.5498(3) 0.4092(3) 0.0242(12) Uani 1 1 d . . . . .
O8 O 0.1537(4) 0.5533(4) 0.4399(4) 0.0328(14) Uani 1 1 d . . . . .
O9 O 0.2114(4) 0.6549(3) 0.3493(3) 0.0297(13) Uani 1 1 d . . . . .
O10 O 0.0964(3) 0.5526(3) 0.2878(3) 0.0258(12) Uani 1 1 d . . . . .
O11 O 0.4842(4) 0.5516(4) 0.3834(4) 0.0313(13) Uani 1 1 d . . . . .
O12 O 0.3686(4) 0.6515(3) 0.3217(3) 0.0276(12) Uani 1 1 d . . . . .
O13 O 0.4175(4) 0.5488(3) 0.2335(3) 0.0263(12) Uani 1 1 d . . . . .
O14 O 0.1504(4) 0.6548(3) 0.2045(3) 0.0271(12) Uani 1 1 d . . . . .
O15 O 0.2655(4) 0.7634(4) 0.2624(4) 0.0396(16) Uani 1 1 d . . . . .
O16 O 0.3104(4) 0.6519(3) 0.1765(3) 0.0281(12) Uani 1 1 d . . . . .
O17 O 0.1990(4) 0.5522(4) 0.1168(3) 0.0305(13) Uani 1 1 d . . . . .
O18 O 0.3666(4) 0.5518(4) 0.0792(4) 0.0386(15) Uani 1 1 d . . . . .
O19 O 0.0277(4) 0.5583(4) 0.1320(4) 0.0382(15) Uani 1 1 d . . . . .
N1 N 0.3615(5) 0.3716(5) 0.5076(5) 0.0354(18) Uani 1 1 d . . . . .
N2 N 0.5105(4) 0.8217(4) 0.3875(4) 0.0286(15) Uani 1 1 d . . . . .
N3 N 0.0380(4) 0.8510(4) 0.1661(4) 0.0233(14) Uani 1 1 d . . . . .
C1 C 0.3429(5) 0.4991(5) 0.4691(5) 0.0286(18) Uani 1 1 d . . . . .
H1C H 0.3073 0.5075 0.5064 0.034 Uiso 1 1 calc R . . . .
H1D H 0.4022 0.5076 0.4922 0.034 Uiso 1 1 calc R . . . .
C2 C 0.2392(5) 0.4051(5) 0.4119(5) 0.0268(17) Uani 1 1 d . . . . .
H2A H 0.2337 0.3547 0.3975 0.032 Uiso 1 1 calc R . . . .
H2B H 0.2046 0.4130 0.4503 0.032 Uiso 1 1 calc R . . . .
C3 C 0.3892(5) 0.4047(5) 0.3860(5) 0.0259(17) Uani 1 1 d . . . . .
H3A H 0.4490 0.4127 0.4077 0.031 Uiso 1 1 calc R . . . .
H3B H 0.3827 0.3542 0.3720 0.031 Uiso 1 1 calc R . . . .
C4 C 0.3332(5) 0.4212(5) 0.4440(5) 0.0274(17) Uani 1 1 d . . . . .
C5 C 0.5267(6) 0.7519(5) 0.3467(5) 0.0332(19) Uani 1 1 d . . . . .
H5A H 0.5276 0.7119 0.3811 0.040 Uiso 1 1 calc R . . . .
H5B H 0.4785 0.7443 0.3065 0.040 Uiso 1 1 calc R . . . .
C6 C 0.6090(7) 0.7498(6) 0.3145(6) 0.044(2) Uani 1 1 d . . . . .
H6A H 0.6583 0.7472 0.3544 0.053 Uiso 1 1 calc R . . . .
H6B H 0.6139 0.7934 0.2860 0.053 Uiso 1 1 calc R . . . .
C7 C 0.6071(8) 0.6827(7) 0.2634(6) 0.049(3) Uani 1 1 d . . . . .
H7A H 0.6641 0.6752 0.2518 0.058 Uiso 1 1 calc R . . . .
H7B H 0.5925 0.6405 0.2901 0.058 Uiso 1 1 calc R . . . .
C8 C 0.5441(9) 0.6896(7) 0.1922(7) 0.056(3) Uani 1 1 d . . . . .
H8A H 0.5470 0.6474 0.1622 0.084 Uiso 1 1 calc GR . . . .
H8B H 0.5578 0.7315 0.1655 0.084 Uiso 1 1 calc GR . . . .
H8C H 0.4870 0.6944 0.2031 0.084 Uiso 1 1 calc GR . . . .
H1A H 0.331(10) 0.364(8) 0.534(8) 0.067 Uiso 1 1 d R . . . .
H1B H 0.439(9) 0.393(8) 0.552(8) 0.067 Uiso 1 1 d R . . . .
C9 C 0.5884(5) 0.8371(5) 0.4473(5) 0.0294(18) Uani 1 1 d . . . . .
H9A H 0.6034 0.7932 0.4756 0.035 Uiso 1 1 calc R . . . .
H9B H 0.6364 0.8495 0.4230 0.035 Uiso 1 1 calc R . . . .
C10 C 0.5767(6) 0.8965(5) 0.5004(5) 0.0315(19) Uani 1 1 d . . . . .
H10A H 0.5317 0.8835 0.5279 0.038 Uiso 1 1 calc R . . . .
H10B H 0.5596 0.9406 0.4729 0.038 Uiso 1 1 calc R . . . .
C11 C 0.6614(6) 0.9092(5) 0.5548(5) 0.035(2) Uani 1 1 d . . . . .
H11A H 0.6768 0.8657 0.5838 0.042 Uiso 1 1 calc R . . . .
H11B H 0.7070 0.9194 0.5269 0.042 Uiso 1 1 calc R . . . .
C12 C 0.6532(7) 0.9718(6) 0.6071(6) 0.044(2) Uani 1 1 d . . . . .
H12A H 0.6493 1.0163 0.5797 0.066 Uiso 1 1 calc GR . . . .
H12B H 0.7027 0.9731 0.6460 0.066 Uiso 1 1 calc GR . . . .
H12C H 0.6024 0.9656 0.6285 0.066 Uiso 1 1 calc GR . . . .
C13 C 0.4973(6) 0.8848(5) 0.3338(5) 0.0322(19) Uani 1 1 d . . . . .
H13A H 0.5453 0.8860 0.3072 0.039 Uiso 1 1 calc R . . . .
H13B H 0.4992 0.9290 0.3626 0.039 Uiso 1 1 calc R . . . .
C14 C 0.4148(6) 0.8846(6) 0.2772(5) 0.035(2) Uani 1 1 d . . . . .
H14A H 0.3660 0.8895 0.3024 0.042 Uiso 1 1 calc R . . . .
H14B H 0.4093 0.8390 0.2505 0.042 Uiso 1 1 calc R . . . .
C15 C 0.4152(6) 0.9471(5) 0.2218(5) 0.033(2) Uani 1 1 d . . . . .
H15A H 0.4407 0.9892 0.2487 0.040 Uiso 1 1 calc R . . . .
H15B H 0.4513 0.9338 0.1861 0.040 Uiso 1 1 calc R . . . .
C16 C 0.3267(6) 0.9670(6) 0.1801(6) 0.041(2) Uani 1 1 d . . . . .
H16A H 0.3324 0.9958 0.1374 0.062 Uiso 1 1 calc GR . . . .
H16B H 0.2966 0.9941 0.2123 0.062 Uiso 1 1 calc GR . . . .
H16C H 0.2952 0.9238 0.1641 0.062 Uiso 1 1 calc GR . . . .
C17 C 0.4289(5) 0.8110(5) 0.4199(5) 0.0290(18) Uani 1 1 d . . . . .
H17A H 0.4142 0.8568 0.4404 0.035 Uiso 1 1 calc R . . . .
H17B H 0.3827 0.7987 0.3796 0.035 Uiso 1 1 calc R . . . .
C18 C 0.4326(6) 0.7537(5) 0.4802(5) 0.0322(19) Uani 1 1 d . . . . .
H18A H 0.4800 0.7638 0.5204 0.039 Uiso 1 1 calc R . . . .
H18B H 0.4419 0.7066 0.4598 0.039 Uiso 1 1 calc R . . . .
C19 C 0.3479(7) 0.7541(6) 0.5097(6) 0.042(2) Uani 1 1 d . . . . .
H19A H 0.3407 0.8009 0.5318 0.050 Uiso 1 1 calc R . . . .
H19B H 0.3008 0.7475 0.4684 0.050 Uiso 1 1 calc R . . . .
C20 C 0.3431(8) 0.6971(6) 0.5660(6) 0.047(3) Uani 1 1 d . . . . .
H20A H 0.3351 0.6510 0.5418 0.071 Uiso 1 1 calc GR . . . .
H20B H 0.2956 0.7068 0.5910 0.071 Uiso 1 1 calc GR . . . .
H20C H 0.3956 0.6967 0.6017 0.071 Uiso 1 1 calc GR . . . .
C21 C 0.1017(5) 0.8506(5) 0.2391(5) 0.0258(17) Uani 1 1 d . . . . .
H21 H 0.107(6) 0.787(6) 0.250(6) 0.031 Uiso 1 1 d R . . . .
C22 C 0.0801(6) 0.8966(5) 0.3017(5) 0.0286(17) Uani 1 1 d . . . . .
H22A H 0.0282 0.8788 0.3172 0.034 Uiso 1 1 calc R . . . .
H22B H 0.0703 0.9462 0.2851 0.034 Uiso 1 1 calc R . . . .
C23 C 0.1554(6) 0.8932(6) 0.3668(5) 0.036(2) Uani 1 1 d . . . . .
H23A H 0.1647 0.8432 0.3821 0.043 Uiso 1 1 calc R . . . .
H23B H 0.2069 0.9099 0.3499 0.043 Uiso 1 1 calc R . . . .
C24 C 0.1429(8) 0.9367(6) 0.4326(6) 0.047(3) Uani 1 1 d . . . . .
H24A H 0.1290 0.9856 0.4174 0.070 Uiso 1 1 calc GR . . . .
H24B H 0.1948 0.9362 0.4690 0.070 Uiso 1 1 calc GR . . . .
H24C H 0.0967 0.9165 0.4540 0.070 Uiso 1 1 calc GR . . . .
C25 C 0.0187(5) 0.9284(4) 0.1404(5) 0.0235(16) Uani 1 1 d . . . . .
H25A H -0.0118 0.9520 0.1755 0.028 Uiso 1 1 calc R . . . .
H25B H -0.0195 0.9273 0.0926 0.028 Uiso 1 1 calc R . . . .
C26 C 0.0972(5) 0.9736(5) 0.1327(5) 0.0281(17) Uani 1 1 d . . . . .
H26A H 0.1327 0.9800 0.1813 0.034 Uiso 1 1 calc R . . . .
H26B H 0.1311 0.9485 0.1012 0.034 Uiso 1 1 calc R . . . .
C27 C 0.0708(6) 1.0461(5) 0.0996(5) 0.0317(19) Uani 1 1 d . . . . .
H27A H 0.0331 1.0696 0.1289 0.038 Uiso 1 1 calc R . . . .
H27B H 0.0391 1.0398 0.0494 0.038 Uiso 1 1 calc R . . . .
C28 C 0.1497(6) 1.0941(5) 0.0974(6) 0.036(2) Uani 1 1 d . . . . .
H28A H 0.1875 1.0705 0.0692 0.053 Uiso 1 1 calc GR . . . .
H28B H 0.1794 1.1024 0.1473 0.053 Uiso 1 1 calc GR . . . .
H28C H 0.1314 1.1395 0.0745 0.053 Uiso 1 1 calc GR . . . .
C29 C 0.0815(5) 0.8092(5) 0.1099(5) 0.0247(16) Uani 1 1 d . . . . .
H29A H 0.1381 0.8297 0.1102 0.030 Uiso 1 1 calc R . . . .
H29B H 0.0895 0.7594 0.1265 0.030 Uiso 1 1 calc R . . . .
C30 C 0.0333(6) 0.8095(5) 0.0314(5) 0.0297(18) Uani 1 1 d . . . . .
H30A H 0.0278 0.8588 0.0133 0.036 Uiso 1 1 calc R . . . .
H30B H -0.0241 0.7905 0.0307 0.036 Uiso 1 1 calc R . . . .
C31 C 0.0778(7) 0.7648(6) -0.0194(5) 0.043(2) Uani 1 1 d . . . . .
H31A H 0.0820 0.7151 -0.0021 0.052 Uiso 1 1 calc R . . . .
H31B H 0.1358 0.7829 -0.0179 0.052 Uiso 1 1 calc R . . . .
C32 C 0.0290(8) 0.7671(6) -0.0998(5) 0.043(2) Uani 1 1 d . . . . .
H32A H 0.0568 0.7359 -0.1303 0.065 Uiso 1 1 calc GR . . . .
H32B H 0.0288 0.8157 -0.1183 0.065 Uiso 1 1 calc GR . . . .
H32C H -0.0291 0.7513 -0.1011 0.065 Uiso 1 1 calc GR . . . .
C33 C -0.0465(5) 0.8156(4) 0.1745(5) 0.0243(16) Uani 1 1 d . . . . .
H33A H -0.0669 0.8381 0.2162 0.029 Uiso 1 1 calc R . . . .
H33B H -0.0883 0.8259 0.1301 0.029 Uiso 1 1 calc R . . . .
C34 C -0.0440(5) 0.7347(5) 0.1866(5) 0.0272(17) Uani 1 1 d . . . . .
H34A H 0.0004 0.7227 0.2287 0.033 Uiso 1 1 calc R . . . .
H34B H -0.0306 0.7106 0.1429 0.033 Uiso 1 1 calc R . . . .
C35 C -0.1319(6) 0.7088(5) 0.2017(5) 0.0317(19) Uani 1 1 d . . . . .
H35A H -0.1411 0.7274 0.2494 0.038 Uiso 1 1 calc R . . . .
H35B H -0.1770 0.7277 0.1635 0.038 Uiso 1 1 calc R . . . .
C36 C -0.1374(6) 0.6264(5) 0.2023(6) 0.037(2) Uani 1 1 d . . . . .
H36A H -0.1341 0.6081 0.1536 0.055 Uiso 1 1 calc GR . . . .
H36B H -0.1909 0.6119 0.2160 0.055 Uiso 1 1 calc GR . . . .
H36C H -0.0905 0.6074 0.2377 0.055 Uiso 1 1 calc GR . . . .
N4 N 0.1925(8) 0.2692(7) 0.0070(8) 0.069(3) Uani 1 1 d . . . . .
C37 C 0.1178(8) 0.3874(7) 0.0347(6) 0.049(3) Uani 1 1 d . . . . .
H37A H 0.0811 0.4031 -0.0100 0.074 Uiso 1 1 calc GR . . . .
H37B H 0.1600 0.4239 0.0510 0.074 Uiso 1 1 calc GR . . . .
H37C H 0.0839 0.3793 0.0728 0.074 Uiso 1 1 calc GR . . . .
C38 C 0.1607(7) 0.3206(6) 0.0203(6) 0.041(2) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0175(5) 0.0212(5) 0.0251(5) 0.0004(4) 0.0035(4) 0.0007(4)
Mo2 0.0153(4) 0.0285(5) 0.0247(4) -0.0024(3) 0.0040(3) -0.0003(3)
Mo3 0.0199(5) 0.0319(6) 0.0354(6) 0.0023(5) 0.0015(4) -0.0002(4)
Mo4 0.0218(5) 0.0206(5) 0.0465(6) 0.0005(4) 0.0008(4) 0.0025(3)
Mo5 0.0256(4) 0.0335(4) 0.0266(4) 0.0036(3) 0.0085(3) 0.0025(3)
Mo6 0.0144(3) 0.0284(4) 0.0271(4) 0.0008(3) -0.0027(3) 0.0012(3)
V1 0.0175(5) 0.0212(5) 0.0251(5) 0.0004(4) 0.0035(4) 0.0007(4)
V2 0.0153(4) 0.0285(5) 0.0247(4) -0.0024(3) 0.0040(3) -0.0003(3)
V3 0.0199(5) 0.0319(6) 0.0354(6) 0.0023(5) 0.0015(4) -0.0002(4)
V4 0.0218(5) 0.0206(5) 0.0465(6) 0.0005(4) 0.0008(4) 0.0025(3)
V5 0.0256(4) 0.0335(4) 0.0266(4) 0.0036(3) 0.0085(3) 0.0025(3)
V6 0.0144(3) 0.0284(4) 0.0271(4) 0.0008(3) -0.0027(3) 0.0012(3)
O1 0.033(3) 0.033(4) 0.041(4) -0.008(3) 0.009(3) -0.005(3)
O2 0.018(3) 0.024(3) 0.026(3) 0.002(2) 0.004(2) -0.001(2)
O3 0.018(3) 0.026(3) 0.029(3) 0.004(2) 0.003(2) -0.001(2)
O4 0.028(3) 0.030(3) 0.029(3) -0.003(2) 0.006(2) 0.001(2)
O5 0.024(3) 0.029(3) 0.028(3) -0.001(2) 0.000(2) 0.000(2)
O6 0.013(2) 0.026(3) 0.025(3) -0.001(2) 0.002(2) 0.001(2)
O7 0.017(3) 0.031(3) 0.023(3) 0.000(2) 0.000(2) -0.003(2)
O8 0.025(3) 0.037(4) 0.037(3) -0.003(3) 0.006(3) -0.001(3)
O9 0.024(3) 0.027(3) 0.038(3) -0.006(3) 0.006(2) 0.001(2)
O10 0.015(3) 0.027(3) 0.035(3) 0.002(2) 0.004(2) -0.001(2)
O11 0.021(3) 0.037(3) 0.034(3) 0.004(3) 0.001(2) -0.004(2)
O12 0.021(3) 0.026(3) 0.035(3) 0.000(2) 0.002(2) -0.005(2)
O13 0.019(3) 0.030(3) 0.032(3) 0.006(2) 0.008(2) 0.003(2)
O14 0.018(3) 0.025(3) 0.036(3) 0.005(2) 0.001(2) 0.008(2)
O15 0.021(3) 0.028(3) 0.068(5) -0.005(3) 0.005(3) 0.000(2)
O16 0.019(3) 0.030(3) 0.035(3) 0.007(2) 0.004(2) 0.001(2)
O17 0.028(3) 0.039(4) 0.023(3) 0.002(2) -0.001(2) 0.002(3)
O18 0.036(4) 0.045(4) 0.037(4) 0.004(3) 0.015(3) 0.006(3)
O19 0.027(3) 0.044(4) 0.040(4) -0.002(3) -0.005(3) 0.003(3)
N1 0.027(4) 0.045(5) 0.033(4) 0.016(4) 0.002(3) 0.004(3)
N2 0.021(3) 0.034(4) 0.030(4) 0.000(3) 0.002(3) -0.006(3)
N3 0.019(3) 0.027(3) 0.024(3) 0.002(3) 0.003(3) 0.006(3)
C1 0.020(4) 0.037(5) 0.026(4) 0.003(3) -0.001(3) -0.005(3)
C2 0.021(4) 0.031(4) 0.027(4) 0.006(3) 0.001(3) -0.003(3)
C3 0.019(4) 0.026(4) 0.031(4) 0.009(3) 0.001(3) 0.006(3)
C4 0.023(4) 0.028(4) 0.029(4) 0.007(3) 0.001(3) 0.001(3)
C5 0.032(5) 0.035(5) 0.034(5) -0.003(4) 0.010(4) -0.007(4)
C6 0.034(5) 0.051(6) 0.048(6) -0.011(5) 0.009(4) 0.001(5)
C7 0.049(6) 0.052(7) 0.051(6) -0.015(5) 0.023(5) -0.004(5)
C8 0.069(8) 0.056(7) 0.047(6) -0.010(5) 0.021(6) -0.010(6)
C9 0.024(4) 0.032(5) 0.033(4) -0.004(4) 0.005(3) -0.005(3)
C10 0.031(4) 0.031(5) 0.033(4) -0.001(4) 0.005(4) -0.003(4)
C11 0.032(5) 0.031(5) 0.039(5) -0.004(4) -0.001(4) 0.001(4)
C12 0.046(6) 0.043(6) 0.039(5) -0.007(4) -0.003(4) -0.004(5)
C13 0.028(4) 0.035(5) 0.034(5) 0.000(4) 0.004(4) -0.012(4)
C14 0.028(4) 0.045(5) 0.032(4) 0.004(4) 0.002(4) -0.012(4)
C15 0.027(4) 0.039(5) 0.033(5) 0.006(4) 0.004(4) -0.004(4)
C16 0.033(5) 0.052(6) 0.038(5) -0.008(5) 0.002(4) -0.005(4)
C17 0.022(4) 0.034(5) 0.031(4) -0.003(4) 0.006(3) -0.006(3)
C18 0.034(5) 0.028(4) 0.036(5) 0.002(4) 0.008(4) -0.003(4)
C19 0.044(6) 0.039(5) 0.047(6) 0.005(4) 0.021(5) 0.003(4)
C20 0.052(7) 0.045(6) 0.050(6) 0.003(5) 0.023(5) -0.008(5)
C21 0.023(4) 0.028(4) 0.024(4) 0.001(3) 0.000(3) 0.003(3)
C22 0.031(4) 0.027(4) 0.027(4) 0.001(3) 0.003(3) 0.001(3)
C23 0.032(5) 0.040(5) 0.034(5) 0.002(4) 0.001(4) -0.002(4)
C24 0.061(7) 0.046(6) 0.029(5) -0.006(4) -0.002(5) 0.000(5)
C25 0.022(4) 0.021(4) 0.026(4) 0.000(3) 0.002(3) 0.007(3)
C26 0.023(4) 0.028(4) 0.033(4) 0.007(3) 0.007(3) 0.009(3)
C27 0.033(5) 0.025(4) 0.036(5) 0.007(4) 0.004(4) 0.002(4)
C28 0.038(5) 0.030(5) 0.040(5) 0.009(4) 0.010(4) 0.003(4)
C29 0.019(4) 0.026(4) 0.030(4) -0.001(3) 0.006(3) 0.005(3)
C30 0.029(4) 0.029(4) 0.032(4) 0.002(3) 0.008(3) 0.002(3)
C31 0.051(6) 0.044(6) 0.033(5) -0.004(4) 0.005(4) 0.019(5)
C32 0.063(7) 0.035(5) 0.032(5) -0.004(4) 0.008(5) 0.013(5)
C33 0.017(4) 0.024(4) 0.032(4) -0.001(3) 0.005(3) 0.006(3)
C34 0.021(4) 0.029(4) 0.031(4) 0.002(3) 0.004(3) 0.002(3)
C35 0.027(4) 0.034(5) 0.036(5) -0.002(4) 0.010(4) 0.000(4)
C36 0.032(5) 0.035(5) 0.042(5) -0.001(4) 0.006(4) -0.005(4)
N4 0.062(7) 0.059(7) 0.090(9) 0.000(6) 0.019(6) -0.015(6)
C37 0.057(7) 0.052(7) 0.041(6) -0.008(5) 0.015(5) -0.013(5)
C38 0.041(6) 0.037(6) 0.044(6) 0.001(4) 0.005(4) -0.011(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 O1 1.614(7) . ?
Mo1 O2 2.067(6) . ?
Mo1 O3 2.063(6) . ?
Mo1 O4 1.818(6) . ?
Mo1 O5 1.830(6) . ?
Mo1 O6 2.225(6) . ?
Mo2 O2 2.100(6) . ?
Mo2 O6 2.224(5) . ?
Mo2 O7 2.080(5) . ?
Mo2 O8 1.646(6) . ?
Mo2 O9 1.797(6) . ?
Mo2 O10 1.825(6) . ?
Mo3 O3 2.034(6) . ?
Mo3 O6 2.231(5) . ?
Mo3 O7 2.028(6) . ?
Mo3 O11 1.615(6) . ?
Mo3 O12 1.803(6) . ?
Mo3 O13 1.847(6) . ?
Mo4 O6 2.330(6) . ?
Mo4 O9 1.972(6) . ?
Mo4 O12 1.908(6) . ?
Mo4 O14 1.908(6) . ?
Mo4 O15 1.632(7) . ?
Mo4 O16 1.870(6) . ?
Mo5 O4 1.952(6) . ?
Mo5 O6 2.384(5) . ?
Mo5 O13 1.883(6) . ?
Mo5 O16 1.887(6) . ?
Mo5 O17 1.949(6) . ?
Mo5 O18 1.668(7) . ?
Mo6 O5 1.952(6) . ?
Mo6 O6 2.346(5) . ?
Mo6 O10 1.988(6) . ?
Mo6 O14 1.889(6) . ?
Mo6 O17 1.868(6) . ?
Mo6 O19 1.666(6) . ?
V1 O1 1.614(7) . ?
V1 O2 2.067(6) . ?
V1 O3 2.063(6) . ?
V1 O4 1.818(6) . ?
V1 O5 1.830(6) . ?
V1 O6 2.225(6) . ?
V2 O2 2.100(6) . ?
V2 O6 2.224(5) . ?
V2 O7 2.080(5) . ?
V2 O8 1.646(6) . ?
V2 O9 1.797(6) . ?
V2 O10 1.825(6) . ?
V3 O3 2.034(6) . ?
V3 O6 2.231(5) . ?
V3 O7 2.028(6) . ?
V3 O11 1.615(6) . ?
V3 O12 1.803(6) . ?
V3 O13 1.847(6) . ?
V4 O6 2.330(6) . ?
V4 O9 1.972(6) . ?
V4 O12 1.908(6) . ?
V4 O14 1.908(6) . ?
V4 O15 1.632(7) . ?
V4 O16 1.870(6) . ?
V5 O4 1.952(6) . ?
V5 O6 2.384(5) . ?
V5 O13 1.883(6) . ?
V5 O16 1.887(6) . ?
V5 O17 1.949(6) . ?
V5 O18 1.668(7) . ?
V6 O5 1.952(6) . ?
V6 O6 2.346(5) . ?
V6 O10 1.988(6) . ?
V6 O14 1.889(6) . ?
V6 O17 1.868(6) . ?
V6 O19 1.666(6) . ?
O2 C2 1.423(10) . ?
O3 C3 1.432(9) . ?
O7 C1 1.439(10) . ?
N1 C4 1.485(11) . ?
N1 H1A 0.75(15) . ?
N1 H1B 1.39(14) . ?
N2 C5 1.535(12) . ?
N2 C9 1.520(11) . ?
N2 C13 1.514(12) . ?
N2 C17 1.521(11) . ?
N3 C21 1.522(10) . ?
N3 C25 1.522(10) . ?
N3 C29 1.540(10) . ?
N3 C33 1.518(10) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C4 1.513(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.527(11) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.525(12) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.519(13) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.551(15) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.498(17) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.498(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.538(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.522(14) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.515(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.536(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.516(13) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.521(12) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.528(13) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.484(14) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21 1.20(10) . ?
C21 C22 1.512(12) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.528(12) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.488(14) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.523(12) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.502(11) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.537(13) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.499(12) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.506(13) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.533(14) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.515(11) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.538(12) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.528(13) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
N4 C38 1.122(16) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C37 C38 1.457(17) . ?
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 O2 95.3(3) . . ?
O1 Mo1 O3 96.8(3) . . ?
O1 Mo1 O4 105.8(3) . . ?
O1 Mo1 O5 105.2(3) . . ?
O1 Mo1 O6 168.8(3) . . ?
O2 Mo1 O6 75.7(2) . . ?
O3 Mo1 O2 80.9(2) . . ?
O3 Mo1 O6 75.4(2) . . ?
O4 Mo1 O2 157.1(3) . . ?
O4 Mo1 O3 87.8(3) . . ?
O4 Mo1 O5 95.7(3) . . ?
O4 Mo1 O6 82.2(2) . . ?
O5 Mo1 O2 87.0(2) . . ?
O5 Mo1 O3 155.8(3) . . ?
O5 Mo1 O6 81.4(2) . . ?
O2 Mo2 O6 75.1(2) . . ?
O7 Mo2 O2 79.8(2) . . ?
O7 Mo2 O6 75.6(2) . . ?
O8 Mo2 O2 94.6(3) . . ?
O8 Mo2 O6 167.3(3) . . ?
O8 Mo2 O7 95.5(3) . . ?
O8 Mo2 O9 106.6(3) . . ?
O8 Mo2 O10 105.4(3) . . ?
O9 Mo2 O2 156.3(2) . . ?
O9 Mo2 O6 82.5(2) . . ?
O9 Mo2 O7 87.6(3) . . ?
O9 Mo2 O10 97.6(3) . . ?
O10 Mo2 O2 86.6(2) . . ?
O10 Mo2 O6 81.7(2) . . ?
O10 Mo2 O7 155.9(2) . . ?
O3 Mo3 O6 75.8(2) . . ?
O7 Mo3 O3 82.2(2) . . ?
O7 Mo3 O6 76.5(2) . . ?
O11 Mo3 O3 97.6(3) . . ?
O11 Mo3 O6 170.6(3) . . ?
O11 Mo3 O7 96.1(3) . . ?
O11 Mo3 O12 104.4(3) . . ?
O11 Mo3 O13 105.2(3) . . ?
O12 Mo3 O3 156.8(2) . . ?
O12 Mo3 O6 81.4(2) . . ?
O12 Mo3 O7 88.1(3) . . ?
O12 Mo3 O13 95.0(3) . . ?
O13 Mo3 O3 86.2(3) . . ?
O13 Mo3 O6 81.3(2) . . ?
O13 Mo3 O7 156.9(2) . . ?
O9 Mo4 O6 76.2(2) . . ?
O12 Mo4 O6 76.7(2) . . ?
O12 Mo4 O9 84.9(3) . . ?
O14 Mo4 O6 78.2(2) . . ?
O14 Mo4 O9 86.0(3) . . ?
O14 Mo4 O12 154.8(3) . . ?
O15 Mo4 O6 176.3(3) . . ?
O15 Mo4 O9 100.7(3) . . ?
O15 Mo4 O12 101.0(3) . . ?
O15 Mo4 O14 103.8(3) . . ?
O15 Mo4 O16 103.6(3) . . ?
O16 Mo4 O6 79.4(2) . . ?
O16 Mo4 O9 155.6(3) . . ?
O16 Mo4 O12 89.0(3) . . ?
O16 Mo4 O14 89.7(3) . . ?
O4 Mo5 O6 75.5(2) . . ?
O13 Mo5 O4 87.0(3) . . ?
O13 Mo5 O6 76.6(2) . . ?
O13 Mo5 O16 88.9(3) . . ?
O13 Mo5 O17 152.8(2) . . ?
O16 Mo5 O4 153.1(3) . . ?
O16 Mo5 O6 77.7(2) . . ?
O16 Mo5 O17 87.4(3) . . ?
O17 Mo5 O4 84.2(3) . . ?
O17 Mo5 O6 76.4(2) . . ?
O18 Mo5 O4 102.3(3) . . ?
O18 Mo5 O6 177.8(3) . . ?
O18 Mo5 O13 103.3(3) . . ?
O18 Mo5 O16 104.6(3) . . ?
O18 Mo5 O17 103.7(3) . . ?
O5 Mo6 O6 75.8(2) . . ?
O5 Mo6 O10 82.9(2) . . ?
O10 Mo6 O6 75.4(2) . . ?
O14 Mo6 O5 153.7(2) . . ?
O14 Mo6 O6 78.2(2) . . ?
O14 Mo6 O10 86.5(3) . . ?
O17 Mo6 O5 88.2(3) . . ?
O17 Mo6 O6 78.8(2) . . ?
O17 Mo6 O10 154.0(2) . . ?
O17 Mo6 O14 91.0(3) . . ?
O19 Mo6 O5 102.5(3) . . ?
O19 Mo6 O6 177.5(3) . . ?
O19 Mo6 O10 102.7(3) . . ?
O19 Mo6 O14 103.3(3) . . ?
O19 Mo6 O17 103.1(3) . . ?
O1 V1 O2 95.3(3) . . ?
O1 V1 O3 96.8(3) . . ?
O1 V1 O4 105.8(3) . . ?
O1 V1 O5 105.2(3) . . ?
O1 V1 O6 168.8(3) . . ?
O2 V1 O6 75.7(2) . . ?
O3 V1 O2 80.9(2) . . ?
O3 V1 O6 75.4(2) . . ?
O4 V1 O2 157.1(3) . . ?
O4 V1 O3 87.8(3) . . ?
O4 V1 O5 95.7(3) . . ?
O4 V1 O6 82.2(2) . . ?
O5 V1 O2 87.0(2) . . ?
O5 V1 O3 155.8(3) . . ?
O5 V1 O6 81.4(2) . . ?
O2 V2 O6 75.1(2) . . ?
O7 V2 O2 79.8(2) . . ?
O7 V2 O6 75.6(2) . . ?
O8 V2 O2 94.6(3) . . ?
O8 V2 O6 167.3(3) . . ?
O8 V2 O7 95.5(3) . . ?
O8 V2 O9 106.6(3) . . ?
O8 V2 O10 105.4(3) . . ?
O9 V2 O2 156.3(2) . . ?
O9 V2 O6 82.5(2) . . ?
O9 V2 O7 87.6(3) . . ?
O9 V2 O10 97.6(3) . . ?
O10 V2 O2 86.6(2) . . ?
O10 V2 O6 81.7(2) . . ?
O10 V2 O7 155.9(2) . . ?
O3 V3 O6 75.8(2) . . ?
O7 V3 O3 82.2(2) . . ?
O7 V3 O6 76.5(2) . . ?
O11 V3 O3 97.6(3) . . ?
O11 V3 O6 170.6(3) . . ?
O11 V3 O7 96.1(3) . . ?
O11 V3 O12 104.4(3) . . ?
O11 V3 O13 105.2(3) . . ?
O12 V3 O3 156.8(2) . . ?
O12 V3 O6 81.4(2) . . ?
O12 V3 O7 88.1(3) . . ?
O12 V3 O13 95.0(3) . . ?
O13 V3 O3 86.2(3) . . ?
O13 V3 O6 81.3(2) . . ?
O13 V3 O7 156.9(2) . . ?
O9 V4 O6 76.2(2) . . ?
O12 V4 O6 76.7(2) . . ?
O12 V4 O9 84.9(3) . . ?
O14 V4 O6 78.2(2) . . ?
O14 V4 O9 86.0(3) . . ?
O14 V4 O12 154.8(3) . . ?
O15 V4 O6 176.3(3) . . ?
O15 V4 O9 100.7(3) . . ?
O15 V4 O12 101.0(3) . . ?
O15 V4 O14 103.8(3) . . ?
O15 V4 O16 103.6(3) . . ?
O16 V4 O6 79.4(2) . . ?
O16 V4 O9 155.6(3) . . ?
O16 V4 O12 89.0(3) . . ?
O16 V4 O14 89.7(3) . . ?
O4 V5 O6 75.5(2) . . ?
O13 V5 O4 87.0(3) . . ?
O13 V5 O6 76.6(2) . . ?
O13 V5 O16 88.9(3) . . ?
O13 V5 O17 152.8(2) . . ?
O16 V5 O4 153.1(3) . . ?
O16 V5 O6 77.7(2) . . ?
O16 V5 O17 87.4(3) . . ?
O17 V5 O4 84.2(3) . . ?
O17 V5 O6 76.4(2) . . ?
O18 V5 O4 102.3(3) . . ?
O18 V5 O6 177.8(3) . . ?
O18 V5 O13 103.3(3) . . ?
O18 V5 O16 104.6(3) . . ?
O18 V5 O17 103.7(3) . . ?
O5 V6 O6 75.8(2) . . ?
O5 V6 O10 82.9(2) . . ?
O10 V6 O6 75.4(2) . . ?
O14 V6 O5 153.7(2) . . ?
O14 V6 O6 78.2(2) . . ?
O14 V6 O10 86.5(3) . . ?
O17 V6 O5 88.2(3) . . ?
O17 V6 O6 78.8(2) . . ?
O17 V6 O10 154.0(2) . . ?
O17 V6 O14 91.0(3) . . ?
O19 V6 O5 102.5(3) . . ?
O19 V6 O6 177.5(3) . . ?
O19 V6 O10 102.7(3) . . ?
O19 V6 O14 103.3(3) . . ?
O19 V6 O17 103.1(3) . . ?
C2 O2 Mo1 118.2(5) . . ?
C2 O2 Mo2 120.6(5) . . ?
C2 O2 V1 118.2(5) . . ?
C2 O2 V2 120.6(5) . . ?
C3 O3 Mo1 118.5(5) . . ?
C3 O3 Mo3 118.9(5) . . ?
C3 O3 V1 118.5(5) . . ?
C3 O3 V3 118.9(5) . . ?
C1 O7 Mo2 119.0(5) . . ?
C1 O7 Mo3 119.2(5) . . ?
C1 O7 V2 119.0(5) . . ?
C1 O7 V3 119.2(5) . . ?
C4 N1 H1A 118(10) . . ?
C4 N1 H1B 113(6) . . ?
H1A N1 H1B 106(10) . . ?
C9 N2 C5 108.9(7) . . ?
C9 N2 C17 112.3(7) . . ?
C13 N2 C5 110.5(7) . . ?
C13 N2 C9 108.7(7) . . ?
C13 N2 C17 108.8(7) . . ?
C17 N2 C5 107.6(7) . . ?
C21 N3 C29 106.0(6) . . ?
C25 N3 C21 109.9(6) . . ?
C25 N3 C29 110.9(6) . . ?
C33 N3 C21 111.6(6) . . ?
C33 N3 C25 107.7(6) . . ?
C33 N3 C29 110.7(6) . . ?
O7 C1 H1C 108.9 . . ?
O7 C1 H1D 108.9 . . ?
O7 C1 C4 113.2(7) . . ?
H1C C1 H1D 107.8 . . ?
C4 C1 H1C 108.9 . . ?
C4 C1 H1D 108.9 . . ?
O2 C2 H2A 109.0 . . ?
O2 C2 H2B 109.0 . . ?
O2 C2 C4 112.8(7) . . ?
H2A C2 H2B 107.8 . . ?
C4 C2 H2A 109.0 . . ?
C4 C2 H2B 109.0 . . ?
O3 C3 H3A 109.1 . . ?
O3 C3 H3B 109.1 . . ?
O3 C3 C4 112.4(6) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
N1 C4 C1 110.6(7) . . ?
N1 C4 C2 108.6(7) . . ?
N1 C4 C3 106.7(7) . . ?
C1 C4 C2 110.0(7) . . ?
C1 C4 C3 111.1(7) . . ?
C3 C4 C2 109.8(7) . . ?
N2 C5 H5A 108.3 . . ?
N2 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
C6 C5 N2 115.8(8) . . ?
C6 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
C5 C6 C7 109.0(9) . . ?
H6A C6 H6B 108.3 . . ?
C7 C6 H6A 109.9 . . ?
C7 C6 H6B 109.9 . . ?
C6 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.8 . . ?
C8 C7 C6 113.1(10) . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C10 C9 N2 115.2(7) . . ?
C10 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
C9 C10 C11 109.8(8) . . ?
H10A C10 H10B 108.2 . . ?
C11 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.1(8) . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13A 108.2 . . ?
N2 C13 H13B 108.2 . . ?
N2 C13 C14 116.4(7) . . ?
H13A C13 H13B 107.4 . . ?
C14 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
C13 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
C13 C14 C15 110.2(7) . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 H14A 109.6 . . ?
C15 C14 H14B 109.6 . . ?
C14 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 C14 113.8(8) . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 H17A 108.2 . . ?
N2 C17 H17B 108.2 . . ?
H17A C17 H17B 107.4 . . ?
C18 C17 N2 116.3(7) . . ?
C18 C17 H17A 108.2 . . ?
C18 C17 H17B 108.2 . . ?
C17 C18 H18A 109.9 . . ?
C17 C18 H18B 109.9 . . ?
C17 C18 C19 109.0(8) . . ?
H18A C18 H18B 108.3 . . ?
C19 C18 H18A 109.9 . . ?
C19 C18 H18B 109.9 . . ?
C18 C19 H19A 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 C18 113.2(9) . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 H21 100(5) . . ?
C22 C21 N3 117.1(7) . . ?
C22 C21 H21 116(5) . . ?
C21 C22 H22A 110.0 . . ?
C21 C22 H22B 110.0 . . ?
C21 C22 C23 108.4(7) . . ?
H22A C22 H22B 108.4 . . ?
C23 C22 H22A 110.0 . . ?
C23 C22 H22B 110.0 . . ?
C22 C23 H23A 108.7 . . ?
C22 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 C22 114.1(9) . . ?
C24 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 108.5 . . ?
N3 C25 H25B 108.5 . . ?
N3 C25 C26 115.0(6) . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 H25A 108.5 . . ?
C26 C25 H25B 108.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
C27 C26 C25 110.8(7) . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C26 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
C26 C27 C28 111.0(8) . . ?
H27A C27 H27B 108.0 . . ?
C28 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 H29A 108.5 . . ?
N3 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
C30 C29 N3 115.0(6) . . ?
C30 C29 H29A 108.5 . . ?
C30 C29 H29B 108.5 . . ?
C29 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
C29 C30 C31 111.8(7) . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 H30A 109.3 . . ?
C31 C30 H30B 109.3 . . ?
C30 C31 H31A 109.4 . . ?
C30 C31 H31B 109.4 . . ?
C30 C31 C32 111.2(8) . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 H31A 109.4 . . ?
C32 C31 H31B 109.4 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 108.3 . . ?
N3 C33 H33B 108.3 . . ?
H33A C33 H33B 107.4 . . ?
C34 C33 N3 116.1(6) . . ?
C34 C33 H33A 108.3 . . ?
C34 C33 H33B 108.3 . . ?
C33 C34 H34A 109.8 . . ?
C33 C34 H34B 109.8 . . ?
C33 C34 C35 109.5(7) . . ?
H34A C34 H34B 108.2 . . ?
C35 C34 H34A 109.8 . . ?
C35 C34 H34B 109.8 . . ?
C34 C35 H35A 109.3 . . ?
C34 C35 H35B 109.3 . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 C34 111.5(8) . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
N4 C38 C37 177.9(14) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C2 C4 70.1(8) . . . . ?
Mo1 O3 C3 C4 -69.8(8) . . . . ?
Mo2 O2 C2 C4 -67.7(8) . . . . ?
Mo2 O7 C1 C4 70.6(8) . . . . ?
Mo3 O3 C3 C4 68.4(8) . . . . ?
Mo3 O7 C1 C4 -66.9(8) . . . . ?
V1 O2 C2 C4 70.1(8) . . . . ?
V1 O3 C3 C4 -69.8(8) . . . . ?
V2 O2 C2 C4 -67.7(8) . . . . ?
V2 O7 C1 C4 70.6(8) . . . . ?
V3 O3 C3 C4 68.4(8) . . . . ?
V3 O7 C1 C4 -66.9(8) . . . . ?
O2 C2 C4 N1 -178.4(7) . . . . ?
O2 C2 C4 C1 60.4(9) . . . . ?
O2 C2 C4 C3 -62.1(9) . . . . ?
O3 C3 C4 N1 179.2(7) . . . . ?
O3 C3 C4 C1 -60.2(9) . . . . ?
O3 C3 C4 C2 61.7(9) . . . . ?
O7 C1 C4 N1 177.8(7) . . . . ?
O7 C1 C4 C2 -62.2(9) . . . . ?
O7 C1 C4 C3 59.5(9) . . . . ?
N2 C5 C6 C7 -169.7(9) . . . . ?
N2 C9 C10 C11 -176.9(7) . . . . ?
N2 C13 C14 C15 -174.0(8) . . . . ?
N2 C17 C18 C19 176.1(8) . . . . ?
N3 C21 C22 C23 -175.4(7) . . . . ?
N3 C25 C26 C27 174.1(7) . . . . ?
N3 C29 C30 C31 -177.4(8) . . . . ?
N3 C33 C34 C35 174.4(7) . . . . ?
C5 N2 C9 C10 -170.2(7) . . . . ?
C5 N2 C13 C14 69.6(10) . . . . ?
C5 N2 C17 C18 65.1(9) . . . . ?
C5 C6 C7 C8 71.3(12) . . . . ?
C9 N2 C5 C6 -54.1(10) . . . . ?
C9 N2 C13 C14 -171.0(8) . . . . ?
C9 N2 C17 C18 -54.7(10) . . . . ?
C9 C10 C11 C12 177.0(8) . . . . ?
C13 N2 C5 C6 65.2(10) . . . . ?
C13 N2 C9 C10 69.3(9) . . . . ?
C13 N2 C17 C18 -175.1(7) . . . . ?
C13 C14 C15 C16 -160.7(9) . . . . ?
C17 N2 C5 C6 -176.1(8) . . . . ?
C17 N2 C9 C10 -51.1(10) . . . . ?
C17 N2 C13 C14 -48.3(10) . . . . ?
C17 C18 C19 C20 176.8(9) . . . . ?
C21 N3 C25 C26 55.2(9) . . . . ?
C21 N3 C29 C30 -174.0(7) . . . . ?
C21 N3 C33 C34 -69.6(9) . . . . ?
C21 C22 C23 C24 179.7(9) . . . . ?
C25 N3 C21 C22 52.2(9) . . . . ?
C25 N3 C29 C30 -54.7(9) . . . . ?
C25 N3 C33 C34 169.7(7) . . . . ?
C25 C26 C27 C28 175.5(8) . . . . ?
C29 N3 C21 C22 172.2(7) . . . . ?
C29 N3 C25 C26 -61.7(9) . . . . ?
C29 N3 C33 C34 48.3(9) . . . . ?
C29 C30 C31 C32 -178.6(9) . . . . ?
C33 N3 C21 C22 -67.2(9) . . . . ?
C33 N3 C25 C26 177.0(7) . . . . ?
C33 N3 C29 C30 64.8(9) . . . . ?
C33 C34 C35 C36 171.1(8) . . . . ?
_iucr_refine_instructions_details
;
hk-5-164-amine.res created by SHELXL-2014/7
TITL hk-5-164-amine_a.res in P2(1)/c
REM Old TITL hk-5-164-amine in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.150, Rweak 0.005, Alpha 0.060, Orientation as input
REM Formula found by SHELXT: N16 C152 O76 V12 Mo12 H332
CELL 1.54184 15.7948 18.5129 18.243 90 100.088 90
ZERR 4 0.0003 0.0003 0.0003 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Mo N O V
UNIT 152 328 12 16 76 12
EADP Mo3 V3
EADP Mo5 V5
EADP Mo6 V6
EADP Mo4 V4
EADP V6 Mo6
EADP Mo1 V1
EADP Mo2 V2
EADP V4 Mo4
EADP V3 Mo3
EADP V5 Mo5
EXYZ V6 Mo6
EXYZ Mo1 V1
EXYZ Mo2 V2
EXYZ V4 Mo4
EXYZ V3 Mo3
EXYZ V5 Mo5
L.S. 8
PLAN 80
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.086900 88.606293
FVAR 0.14021
PART 5
MO1 3 0.251756 0.430194 0.251063 10.25000 0.01751 0.02122 =
0.02512 0.00044 0.00351 0.00070
PART 0
PART 7
MO2 3 0.190602 0.560592 0.361244 10.50000 0.01528 0.02849 =
0.02467 -0.00241 0.00399 -0.00030
PART 0
PART 12
MO3 3 0.392446 0.556267 0.328322 10.25000 0.01988 0.03195 =
0.03542 0.00230 0.00147 -0.00018
PART 0
PART 10
MO4 3 0.261850 0.675297 0.259912 10.50000 0.02176 0.02056 =
0.04652 0.00049 0.00079 0.00253
PART 0
PART 14
MO5 3 0.322068 0.552988 0.155625 10.75000 0.02562 0.03352 =
0.02656 0.00363 0.00853 0.00247
PART 0
PART 4
MO6 3 0.124494 0.556129 0.185764 10.75000 0.01440 0.02838 =
0.02711 0.00081 -0.00273 0.00124
PART 0
PART 6
V1 6 0.251756 0.430194 0.251063 10.75000 0.01751 0.02122 =
0.02512 0.00044 0.00351 0.00070
PART 0
PART 8
V2 6 0.190602 0.560592 0.361244 10.50000 0.01528 0.02849 =
0.02467 -0.00241 0.00399 -0.00030
PART 0
PART 11
V3 6 0.392446 0.556267 0.328322 10.75000 0.01988 0.03195 =
0.03542 0.00230 0.00147 -0.00018
PART 0
PART 9
V4 6 0.261850 0.675297 0.259912 10.50000 0.02176 0.02056 =
0.04652 0.00049 0.00079 0.00253
PART 0
PART 13
V5 6 0.322068 0.552988 0.155625 10.25000 0.02562 0.03352 =
0.02656 0.00363 0.00853 0.00247
PART 0
PART 3
V6 6 0.124494 0.556129 0.185764 10.25000 0.01440 0.02838 =
0.02711 0.00081 -0.00273 0.00124
PART 0
O1 5 0.252599 0.343293 0.258487 11.00000 0.03326 0.03270 =
0.04130 -0.00757 0.00870 -0.00510
O2 5 0.206711 0.448869 0.349106 11.00000 0.01794 0.02419 =
0.02581 0.00244 0.00400 -0.00065
O3 5 0.367481 0.448509 0.320742 11.00000 0.01831 0.02573 =
0.02936 0.00380 0.00278 -0.00061
O4 5 0.305664 0.450343 0.173185 11.00000 0.02836 0.03033 =
0.02881 -0.00270 0.00575 0.00094
O5 5 0.143604 0.452792 0.202418 11.00000 0.02369 0.02863 =
0.02774 -0.00130 0.00018 0.00034
O6 5 0.258467 0.549587 0.264838 11.00000 0.01288 0.02594 =
0.02547 -0.00075 0.00194 0.00082
O7 5 0.319514 0.549819 0.409186 11.00000 0.01666 0.03130 =
0.02325 0.00008 -0.00028 -0.00316
O8 5 0.153680 0.553345 0.439888 11.00000 0.02482 0.03740 =
0.03660 -0.00326 0.00632 -0.00103
O9 5 0.211396 0.654930 0.349278 11.00000 0.02432 0.02706 =
0.03801 -0.00588 0.00632 0.00079
O10 5 0.096447 0.552602 0.287797 11.00000 0.01529 0.02710 =
0.03503 0.00243 0.00436 -0.00070
O11 5 0.484226 0.551617 0.383354 11.00000 0.02143 0.03676 =
0.03406 0.00410 0.00068 -0.00399
O12 5 0.368557 0.651532 0.321733 11.00000 0.02080 0.02629 =
0.03471 -0.00034 0.00216 -0.00537
O13 5 0.417547 0.548805 0.233454 11.00000 0.01853 0.02994 =
0.03180 0.00621 0.00778 0.00280
O14 5 0.150424 0.654761 0.204543 11.00000 0.01827 0.02519 =
0.03624 0.00503 0.00054 0.00762
O15 5 0.265461 0.763406 0.262357 11.00000 0.02101 0.02845 =
0.06809 -0.00502 0.00463 0.00008
O16 5 0.310368 0.651949 0.176493 11.00000 0.01925 0.03015 =
0.03469 0.00749 0.00438 0.00097
O17 5 0.198993 0.552183 0.116803 11.00000 0.02750 0.03947 =
0.02262 0.00201 -0.00093 0.00193
O18 5 0.366633 0.551830 0.079241 11.00000 0.03633 0.04534 =
0.03707 0.00388 0.01455 0.00553
O19 5 0.027699 0.558347 0.132045 11.00000 0.02719 0.04379 =
0.03978 -0.00183 -0.00498 0.00310
N1 4 0.361477 0.371601 0.507634 11.00000 0.02665 0.04534 =
0.03307 0.01639 0.00225 0.00399
N2 4 0.510503 0.821732 0.387542 11.00000 0.02114 0.03412 =
0.02986 0.00041 0.00228 -0.00588
N3 4 0.037992 0.850975 0.166112 11.00000 0.01876 0.02660 =
0.02411 0.00248 0.00261 0.00608
C1 1 0.342946 0.499107 0.469101 11.00000 0.02031 0.03730 =
0.02625 0.00334 -0.00136 -0.00511
AFIX 23
H1C 2 0.307259 0.507546 0.506450 11.00000 -1.20000
H1D 2 0.402247 0.507562 0.492176 11.00000 -1.20000
AFIX 0
C2 1 0.239160 0.405142 0.411937 11.00000 0.02054 0.03118 =
0.02742 0.00574 0.00108 -0.00337
AFIX 23
H2A 2 0.233660 0.354705 0.397484 11.00000 -1.20000
H2B 2 0.204627 0.413024 0.450251 11.00000 -1.20000
AFIX 0
C3 1 0.389202 0.404714 0.386007 11.00000 0.01940 0.02644 =
0.03055 0.00892 0.00081 0.00625
AFIX 23
H3A 2 0.449023 0.412744 0.407750 11.00000 -1.20000
H3B 2 0.382662 0.354212 0.371988 11.00000 -1.20000
AFIX 0
C4 1 0.333170 0.421170 0.444048 11.00000 0.02315 0.02845 =
0.02933 0.00697 0.00099 0.00096
C5 1 0.526669 0.751943 0.346708 11.00000 0.03181 0.03530 =
0.03392 -0.00324 0.00952 -0.00680
AFIX 23
H5A 2 0.527572 0.711886 0.381111 11.00000 -1.20000
H5B 2 0.478533 0.744339 0.306483 11.00000 -1.20000
AFIX 0
C6 1 0.609001 0.749838 0.314485 11.00000 0.03418 0.05106 =
0.04751 -0.01056 0.00881 0.00136
AFIX 23
H6A 2 0.658321 0.747243 0.354411 11.00000 -1.20000
H6B 2 0.613922 0.793429 0.286029 11.00000 -1.20000
AFIX 0
C7 1 0.607087 0.682702 0.263402 11.00000 0.04853 0.05166 =
0.05054 -0.01490 0.02272 -0.00391
AFIX 23
H7A 2 0.664086 0.675170 0.251845 11.00000 -1.20000
H7B 2 0.592484 0.640500 0.290137 11.00000 -1.20000
AFIX 0
C8 1 0.544065 0.689614 0.192156 11.00000 0.06861 0.05576 =
0.04748 -0.00995 0.02125 -0.01020
AFIX 137
H8A 2 0.546983 0.647350 0.162210 11.00000 -1.50000
H8B 2 0.557787 0.731526 0.165542 11.00000 -1.50000
H8C 2 0.487031 0.694397 0.203052 11.00000 -1.50000
AFIX 0
H1A 2 0.330862 0.364437 0.533885 11.00000 -1.20000
H1B 2 0.438661 0.392776 0.551689 11.00000 -1.20000
C9 1 0.588357 0.837145 0.447261 11.00000 0.02390 0.03178 =
0.03255 -0.00394 0.00461 -0.00545
AFIX 23
H9A 2 0.603445 0.793250 0.475579 11.00000 -1.20000
H9B 2 0.636412 0.849456 0.423035 11.00000 -1.20000
AFIX 0
C10 1 0.576715 0.896516 0.500369 11.00000 0.03064 0.03130 =
0.03268 -0.00141 0.00546 -0.00304
AFIX 23
H10A 2 0.531666 0.883548 0.527880 11.00000 -1.20000
H10B 2 0.559638 0.940554 0.472917 11.00000 -1.20000
AFIX 0
C11 1 0.661420 0.909151 0.554822 11.00000 0.03194 0.03094 =
0.03916 -0.00428 -0.00119 0.00051
AFIX 23
H11A 2 0.676816 0.865680 0.583782 11.00000 -1.20000
H11B 2 0.706986 0.919377 0.526936 11.00000 -1.20000
AFIX 0
C12 1 0.653194 0.971832 0.607070 11.00000 0.04611 0.04295 =
0.03897 -0.00678 -0.00258 -0.00407
AFIX 137
H12A 2 0.649299 1.016342 0.579686 11.00000 -1.50000
H12B 2 0.702740 0.973089 0.645951 11.00000 -1.50000
H12C 2 0.602355 0.965610 0.628537 11.00000 -1.50000
AFIX 0
C13 1 0.497332 0.884760 0.333829 11.00000 0.02756 0.03516 =
0.03357 0.00048 0.00422 -0.01200
AFIX 23
H13A 2 0.545328 0.886038 0.307172 11.00000 -1.20000
H13B 2 0.499206 0.928974 0.362599 11.00000 -1.20000
AFIX 0
C14 1 0.414835 0.884566 0.277164 11.00000 0.02765 0.04495 =
0.03165 0.00385 0.00212 -0.01191
AFIX 23
H14A 2 0.365998 0.889548 0.302448 11.00000 -1.20000
H14B 2 0.409268 0.839006 0.250494 11.00000 -1.20000
AFIX 0
C15 1 0.415236 0.947072 0.221843 11.00000 0.02662 0.03913 =
0.03320 0.00564 0.00367 -0.00352
AFIX 23
H15A 2 0.440681 0.989181 0.248739 11.00000 -1.20000
H15B 2 0.451297 0.933823 0.186063 11.00000 -1.20000
AFIX 0
C16 1 0.326748 0.967034 0.180103 11.00000 0.03309 0.05208 =
0.03771 -0.00769 0.00185 -0.00531
AFIX 137
H16A 2 0.332446 0.995780 0.137440 11.00000 -1.50000
H16B 2 0.296554 0.994122 0.212281 11.00000 -1.50000
H16C 2 0.295194 0.923844 0.164149 11.00000 -1.50000
AFIX 0
C17 1 0.428940 0.811040 0.419937 11.00000 0.02188 0.03417 =
0.03127 -0.00264 0.00566 -0.00618
AFIX 23
H17A 2 0.414187 0.856784 0.440374 11.00000 -1.20000
H17B 2 0.382658 0.798663 0.379557 11.00000 -1.20000
AFIX 0
C18 1 0.432642 0.753737 0.480192 11.00000 0.03384 0.02759 =
0.03592 0.00248 0.00829 -0.00308
AFIX 23
H18A 2 0.480037 0.763770 0.520415 11.00000 -1.20000
H18B 2 0.441920 0.706580 0.459816 11.00000 -1.20000
AFIX 0
C19 1 0.347893 0.754132 0.509733 11.00000 0.04429 0.03856 =
0.04655 0.00461 0.02062 0.00283
AFIX 23
H19A 2 0.340658 0.800921 0.531759 11.00000 -1.20000
H19B 2 0.300817 0.747542 0.468357 11.00000 -1.20000
AFIX 0
C20 1 0.343133 0.697121 0.566048 11.00000 0.05240 0.04479 =
0.04951 0.00327 0.02280 -0.00848
AFIX 137
H20A 2 0.335086 0.650964 0.541845 11.00000 -1.50000
H20B 2 0.295643 0.706841 0.590988 11.00000 -1.50000
H20C 2 0.395591 0.696676 0.601742 11.00000 -1.50000
AFIX 0
C21 1 0.101729 0.850559 0.239087 11.00000 0.02340 0.02805 =
0.02449 0.00144 -0.00008 0.00333
H21 2 0.106706 0.786680 0.250290 11.00000 -1.20000
C22 1 0.080098 0.896600 0.301743 11.00000 0.03072 0.02682 =
0.02733 0.00081 0.00278 0.00105
AFIX 23
H22A 2 0.028215 0.878775 0.317199 11.00000 -1.20000
H22B 2 0.070266 0.946154 0.285149 11.00000 -1.20000
AFIX 0
C23 1 0.155409 0.893167 0.366848 11.00000 0.03193 0.04017 =
0.03358 0.00232 0.00129 -0.00220
AFIX 23
H23A 2 0.164744 0.843183 0.382082 11.00000 -1.20000
H23B 2 0.206883 0.909944 0.349914 11.00000 -1.20000
AFIX 0
C24 1 0.142859 0.936723 0.432641 11.00000 0.06139 0.04615 =
0.02926 -0.00586 -0.00213 -0.00041
AFIX 137
H24A 2 0.128971 0.985571 0.417430 11.00000 -1.50000
H24B 2 0.194776 0.936204 0.468983 11.00000 -1.50000
H24C 2 0.096733 0.916497 0.453965 11.00000 -1.50000
AFIX 0
C25 1 0.018662 0.928352 0.140364 11.00000 0.02223 0.02133 =
0.02617 0.00046 0.00218 0.00711
AFIX 23
H25A 2 -0.011761 0.952033 0.175464 11.00000 -1.20000
H25B 2 -0.019538 0.927259 0.092552 11.00000 -1.20000
AFIX 0
C26 1 0.097200 0.973581 0.132727 11.00000 0.02326 0.02840 =
0.03338 0.00715 0.00683 0.00865
AFIX 23
H26A 2 0.132691 0.980033 0.181341 11.00000 -1.20000
H26B 2 0.131100 0.948461 0.101230 11.00000 -1.20000
AFIX 0
C27 1 0.070757 1.046126 0.099568 11.00000 0.03333 0.02457 =
0.03643 0.00696 0.00424 0.00169
AFIX 23
H27A 2 0.033105 1.069624 0.128907 11.00000 -1.20000
H27B 2 0.039066 1.039791 0.049418 11.00000 -1.20000
AFIX 0
C28 1 0.149656 1.094125 0.097441 11.00000 0.03772 0.03034 =
0.03956 0.00883 0.00953 0.00270
AFIX 137
H28A 2 0.187477 1.070467 0.069215 11.00000 -1.50000
H28B 2 0.179427 1.102409 0.147283 11.00000 -1.50000
H28C 2 0.131358 1.139488 0.074497 11.00000 -1.50000
AFIX 0
C29 1 0.081522 0.809156 0.109897 11.00000 0.01928 0.02567 =
0.02999 -0.00087 0.00633 0.00525
AFIX 23
H29A 2 0.138091 0.829673 0.110200 11.00000 -1.20000
H29B 2 0.089462 0.759447 0.126484 11.00000 -1.20000
AFIX 0
C30 1 0.033272 0.809455 0.031432 11.00000 0.02929 0.02875 =
0.03199 0.00219 0.00783 0.00213
AFIX 23
H30A 2 0.027799 0.858772 0.013261 11.00000 -1.20000
H30B 2 -0.024145 0.790541 0.030685 11.00000 -1.20000
AFIX 0
C31 1 0.077842 0.764767 -0.019421 11.00000 0.05087 0.04445 =
0.03269 -0.00402 0.00525 0.01863
AFIX 23
H31A 2 0.081954 0.715131 -0.002133 11.00000 -1.20000
H31B 2 0.135752 0.782893 -0.017860 11.00000 -1.20000
AFIX 0
C32 1 0.029031 0.767136 -0.099786 11.00000 0.06257 0.03474 =
0.03221 -0.00372 0.00797 0.01289
AFIX 137
H32A 2 0.056800 0.735945 -0.130317 11.00000 -1.50000
H32B 2 0.028794 0.815695 -0.118285 11.00000 -1.50000
H32C 2 -0.029071 0.751250 -0.101086 11.00000 -1.50000
AFIX 0
C33 1 -0.046498 0.815643 0.174488 11.00000 0.01718 0.02430 =
0.03170 -0.00076 0.00507 0.00612
AFIX 23
H33A 2 -0.066926 0.838107 0.216160 11.00000 -1.20000
H33B 2 -0.088306 0.825950 0.130099 11.00000 -1.20000
AFIX 0
C34 1 -0.044015 0.734651 0.186642 11.00000 0.02144 0.02873 =
0.03118 0.00218 0.00384 0.00214
AFIX 23
H34A 2 0.000415 0.722676 0.228667 11.00000 -1.20000
H34B 2 -0.030560 0.710556 0.142881 11.00000 -1.20000
AFIX 0
C35 1 -0.131892 0.708782 0.201688 11.00000 0.02668 0.03377 =
0.03621 -0.00171 0.00968 -0.00013
AFIX 23
H35A 2 -0.141098 0.727419 0.249363 11.00000 -1.20000
H35B 2 -0.176956 0.727732 0.163521 11.00000 -1.20000
AFIX 0
C36 1 -0.137356 0.626381 0.202300 11.00000 0.03239 0.03545 =
0.04195 -0.00065 0.00569 -0.00452
AFIX 137
H36A 2 -0.134141 0.608081 0.153627 11.00000 -1.50000
H36B 2 -0.190866 0.611939 0.215954 11.00000 -1.50000
H36C 2 -0.090495 0.607354 0.237704 11.00000 -1.50000
AFIX 0
N4 4 0.192530 0.269162 0.007025 11.00000 0.06162 0.05854 =
0.09000 -0.00029 0.01920 -0.01472
C37 1 0.117757 0.387409 0.034742 11.00000 0.05699 0.05219 =
0.04083 -0.00798 0.01488 -0.01321
AFIX 137
H37A 2 0.081067 0.403069 -0.010046 11.00000 -1.50000
H37B 2 0.160033 0.423938 0.050971 11.00000 -1.50000
H37C 2 0.083880 0.379259 0.072812 11.00000 -1.50000
AFIX 0
C38 1 0.160701 0.320562 0.020306 11.00000 0.04148 0.03723 =
0.04420 0.00100 0.00458 -0.01131
HKLF 4
REM hk-5-164-amine_a.res in P2(1)/c
REM R1 = 0.0693 for 9429 Fo > 4sig(Fo) and 0.0758 for all 10711 data
REM 622 parameters refined using 0 restraints
END
WGHT 0.0869 88.6510
REM Highest difference peak 1.410, deepest hole -1.696, 1-sigma level 0.215
Q1 1 0.2500 0.6606 0.3094 11.00000 0.05 1.41
Q2 1 0.3171 0.5524 0.2100 11.00000 0.05 1.40
Q3 1 0.3844 0.5575 0.3819 11.00000 0.05 1.34
Q4 1 0.1198 0.6413 0.2336 11.00000 0.05 1.25
Q5 1 0.1936 0.5563 0.4115 11.00000 0.05 1.24
Q6 1 0.1130 0.5432 0.2389 11.00000 0.05 1.22
Q7 1 0.3895 0.6138 0.3488 11.00000 0.05 1.20
Q8 1 0.1922 0.6201 0.3685 11.00000 0.05 1.19
Q9 1 0.6716 0.7793 0.3317 11.00000 0.05 1.18
Q10 1 0.2514 0.5019 0.2467 11.00000 0.05 1.18
Q11 1 0.7331 0.6611 0.2263 11.00000 0.05 1.17
Q12 1 0.1298 0.6177 0.1974 11.00000 0.05 1.15
Q13 1 0.2516 0.8780 0.2458 11.00000 0.05 1.15
Q14 1 -0.1843 0.7803 0.1390 11.00000 0.05 1.13
Q15 1 0.3295 0.6182 0.1709 11.00000 0.05 1.12
Q16 1 0.2769 0.7415 0.3074 11.00000 0.05 1.12
Q17 1 0.2886 0.6421 0.2066 11.00000 0.05 1.10
Q18 1 0.3182 0.7319 0.6542 11.00000 0.05 1.05
Q19 1 0.1863 0.7735 0.3653 11.00000 0.05 1.00
Q20 1 0.1528 0.8722 0.2242 11.00000 0.05 0.97
Q21 1 -0.1272 0.7751 0.3060 11.00000 0.05 0.97
Q22 1 0.2450 0.4276 0.3055 11.00000 0.05 0.96
Q23 1 0.6123 0.7804 0.1618 11.00000 0.05 0.91
Q24 1 0.3433 0.5389 0.1069 11.00000 0.05 0.89
Q25 1 0.4275 0.5517 0.2775 11.00000 0.05 0.88
Q26 1 0.5734 0.7871 0.2731 11.00000 0.05 0.86
Q27 1 0.2301 0.5416 0.3093 11.00000 0.05 0.84
Q28 1 0.6361 0.6817 0.1584 11.00000 0.05 0.79
Q29 1 0.3899 0.7730 0.3385 11.00000 0.05 0.79
Q30 1 0.1200 0.7655 0.1766 11.00000 0.05 0.77
Q31 1 0.2641 0.4137 0.1999 11.00000 0.05 0.76
Q32 1 0.2448 0.7476 0.2503 11.00000 0.05 0.76
Q33 1 0.0708 0.5924 0.1083 11.00000 0.05 0.75
Q34 1 0.0546 0.5345 0.3190 11.00000 0.05 0.74
Q35 1 0.1429 0.5522 0.1329 11.00000 0.05 0.71
Q36 1 0.3035 0.5287 0.2529 11.00000 0.05 0.68
Q37 1 0.4513 0.8605 0.2436 11.00000 0.05 0.68
Q38 1 0.3626 0.6500 0.3604 11.00000 0.05 0.68
Q39 1 0.1588 0.5804 0.1494 11.00000 0.05 0.67
Q40 1 0.3286 0.7066 0.2591 11.00000 0.05 0.67
Q41 1 0.3058 0.6956 0.2185 11.00000 0.05 0.66
Q42 1 0.4111 0.6474 0.2753 11.00000 0.05 0.63
Q43 1 0.2574 0.2886 0.2748 11.00000 0.05 0.63
Q44 1 0.0436 0.6066 0.1816 11.00000 0.05 0.61
Q45 1 0.3017 0.3914 0.1461 11.00000 0.05 0.61
Q46 1 -0.0789 0.7883 0.2189 11.00000 0.05 0.60
Q47 1 0.1368 0.5155 0.1968 11.00000 0.05 0.59
Q48 1 0.0497 0.7420 -0.2034 11.00000 0.05 0.57
Q49 1 0.3546 0.5077 0.3107 11.00000 0.05 0.56
Q50 1 0.4045 0.3897 0.5440 11.00000 0.05 0.54
Q51 1 -0.0103 0.8974 0.2103 11.00000 0.05 0.53
Q52 1 0.4045 0.8462 0.5508 11.00000 0.05 0.52
Q53 1 0.0198 0.8722 0.2415 11.00000 0.05 0.52
Q54 1 0.6741 0.6503 0.2847 11.00000 0.05 0.52
Q55 1 0.4590 0.5885 0.4142 11.00000 0.05 0.51
Q56 1 -0.1989 0.6795 0.1703 11.00000 0.05 0.51
Q57 1 0.6831 0.6816 0.3147 11.00000 0.05 0.49
Q58 1 0.3480 0.5057 0.2412 11.00000 0.05 0.48
Q59 1 0.4996 0.4276 0.5414 11.00000 0.05 0.48
Q60 1 0.6403 0.9226 0.6845 11.00000 0.05 0.47
Q61 1 0.6410 0.7536 0.2643 11.00000 0.05 0.47
Q62 1 0.2042 1.1480 0.1767 11.00000 0.05 0.47
Q63 1 0.0772 1.0062 0.1144 11.00000 0.05 0.46
Q64 1 0.3310 0.8770 0.4461 11.00000 0.05 0.46
Q65 1 0.3604 0.6217 0.2357 11.00000 0.05 0.46
Q66 1 0.2189 0.7291 0.4007 11.00000 0.05 0.46
Q67 1 0.4723 0.3993 0.5846 11.00000 0.05 0.46
Q68 1 0.1645 0.7416 0.0652 11.00000 0.05 0.45
Q69 1 0.1704 0.7317 0.0118 11.00000 0.05 0.45
Q70 1 0.0418 0.8887 0.3927 11.00000 0.05 0.45
Q71 1 0.6132 0.5742 0.2514 11.00000 0.05 0.45
Q72 1 0.3516 0.4291 0.3823 11.00000 0.05 0.45
Q73 1 0.0931 0.5802 0.4826 11.00000 0.05 0.45
Q74 1 0.4504 0.9007 0.1948 11.00000 0.05 0.45
Q75 1 0.6309 0.6066 0.2441 11.00000 0.05 0.45
Q76 1 -0.0217 0.5504 0.1725 11.00000 0.05 0.45
Q77 1 0.1689 0.7527 0.0873 11.00000 0.05 0.45
Q78 1 0.2966 0.6103 0.0727 11.00000 0.05 0.44
Q79 1 0.2598 0.5900 0.3991 11.00000 0.05 0.44
Q80 1 0.0769 0.8803 0.2620 11.00000 0.05 0.44
REM The information below was added by Olex2.
REM
REM R1 = 0.0693 for 9429 Fo > 4sig(Fo) and 0.0758 for all 33144 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.41, deepest hole -1.70
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0758
REM R1_gt = 0.0693
REM wR_ref = 0.2465
REM GOOF = 1.157
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 33144
REM Reflections_gt = 9429
REM Parameters = n/a
REM Hole = -1.70
REM Peak = 1.41
REM Flack = n/a
;
_olex2_date_sample_data_collection 2017-03-16
_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 2.191
_oxdiff_exptl_absorpt_empirical_full_min 0.474