#------------------------------------------------------------------------------
#$Date: 2022-05-05 23:25:36 +0300 (Thu, 05 May 2022) $
#$Revision: 274963 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/63/1566333.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1566333
loop_
_publ_author_name
'Salazar Marcano, David E.'
'Moussawi, Mhamad Aly'
'Anyushin, Alexander V.'
'Lentink, Sarah'
'Van Meervelt, Luc'
'Ivanović-Burmazović, Ivana'
'Parac-Vogt, Tatjana N'
_publ_section_title
;
 Versatile post-functionalisation strategy for the formation of modular
 organic-inorganic polyoxometalate hybrids.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2891
_journal_page_last               2899
_journal_paper_doi               10.1039/d1sc06326j
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C10 H19 O13.5 V3, C16 H36 N'
_chemical_formula_sum            'C26 H55 N O13.5 V3'
_chemical_formula_weight         750.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-06 deposited with the CCDC.	2022-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.803(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0520(12)
_cell_length_b                   13.4949(9)
_cell_length_c                   20.5929(10)
_cell_measurement_reflns_used    6373
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.9150
_cell_measurement_theta_min      2.8970
_cell_volume                     3506.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9631
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -93.00 -35.00   1.00   30.00    --  -17.07-178.00 -90.00   58
  2  ω    -90.00  56.00   1.00   30.00    --  -17.07   0.00 150.00  146
  3  ω     34.00  95.00   1.00   30.00    --   18.87-178.00   0.00   61
  4  ω    -87.00  13.00   1.00   30.00    --  -17.07 -77.00  90.00  100
  5  ω    -20.00  25.00   1.00   30.00    --  -17.07 -99.00 -60.00   45
  6  ω    -43.00  55.00   1.00   30.00    --  -17.07  38.00-150.00   98
  7  ω    -20.00  13.00   1.00   30.00    --   18.87 -99.00  90.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0463760000
_diffrn_orient_matrix_UB_12      -0.0103474000
_diffrn_orient_matrix_UB_13      -0.0257816000
_diffrn_orient_matrix_UB_21      -0.0228187000
_diffrn_orient_matrix_UB_22      0.0451344000
_diffrn_orient_matrix_UB_23      0.0070347000
_diffrn_orient_matrix_UB_31      0.0221896000
_diffrn_orient_matrix_UB_32      0.0248215000
_diffrn_orient_matrix_UB_33      -0.0235505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            38832
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.542
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         5912
_refine_ls_number_restraints     445
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0857
_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/[σ²(Fo²)+(0.0966P)²+8.4208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2097
_refine_ls_wR_factor_ref         0.2460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3732
_reflns_number_total             5912
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc06326j2.cif
_cod_data_source_block           tpv2008_tw
_cod_depositor_comments
'Adding full bibliography for 1566332--1566333.cif.'
_cod_original_cell_volume        3506.8(4)
_cod_original_formula_sum        'C26 H55 N O13.50 V3'
_cod_database_code               1566333
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C52H110N2O27V6
_chemical_oxdiff_usercomment     AA0070-MeOH+AcN/Et2O
_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.
;
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.786
_diffrn_oxdiff_ac4_digest_frames
;
011a00f3b689db7b124c9d8401d335b91f000273ff1
;
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.766(4)
 0.234(4)
2. 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
3. Restrained distances
 N28-C29 = N28-C33 = N28-C37 = N28-C41
 1.521 with sigma of 0.02
 C29-C30 = C33-C34 = C37-C38 = C41-C42
 1.511 with sigma of 0.02
 C30-C31 = C34-C35 = C38-C39 = C42-C43A = C42-C43B
 1.525 with sigma of 0.02
 C31-C32 = C35-C36 = C39-C40A = C39-C40B = C43A-C44A = C43B-C44B
 1.487 with sigma of 0.02
 N28-C30 = N28-C34 = N28-C38 = N28-C42
 2.568 with sigma of 0.04
 C29-C31 = C33-C35 = C37-C39 = C41-C43A = C41-C43B
 2.497 with sigma of 0.04
 C30-C32 = C34-C36 = C38-C40A = C38-C40B = C42-C44A = C42-C44B
 2.503 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C40A) = Uanis(C40B)
Uanis(C43A) = Uanis(C43B)
Uanis(C44A) = Uanis(C44B)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44D)=
 Sof(H44E)=Sof(H44F)=1-FVAR(2)
 Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C44A)=Sof(H44A)=
 Sof(H44B)=Sof(H44C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,
 H20B), C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C39(H39C,H39D), C41(H41A,
 H41B), C42(H42A,H42B), C42(H42C,H42D), C43A(H43A,H43B), C43B(H43C,H43D)
7.b Me refined with riding coordinates:
 C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F)
7.c Tetrahedral OH refined with riding coordinates:
 O25(H25)
7.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C40A(H40A,H40B,H40C), C40B(H40D,
 H40E,H40F)
7.e Idealised tetrahedral OH refined as rotating group:
 O23(H23), O27(H27)
;
_olex2_submission_original_sample_id 'AA0070 MeOH + ACN/Et2O'
_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 4.191
_oxdiff_exptl_absorpt_empirical_full_min 0.489
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'
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
V1 V 0.64713(10) 0.48155(10) 0.58271(6) 0.0565(4) Uani 1 1 d . U . . .
O2 O 0.7055(4) 0.5130(3) 0.5043(2) 0.0539(11) Uani 1 1 d . U . . .
V3 V 0.58483(10) 0.51945(9) 0.41900(5) 0.0529(4) Uani 1 1 d . U . . .
O4 O 0.5850(4) 0.3823(3) 0.4234(2) 0.0556(12) Uani 1 1 d . U . . .
V5 V 0.51526(11) 0.33715(9) 0.48254(6) 0.0573(4) Uani 1 1 d . U . . .
O6 O 0.6322(4) 0.3537(3) 0.5560(2) 0.0609(12) Uani 1 1 d . U . . .
O7 O 0.500000 0.500000 0.500000 0.0470(14) Uani 1 2 d S TU P . .
O8 O 0.5111(5) 0.2199(4) 0.4712(3) 0.0766(16) Uani 1 1 d . U . . .
O9 O 0.7581(4) 0.4821(4) 0.6379(3) 0.0731(15) Uani 1 1 d . U . . .
O10 O 0.6239(4) 0.6292(4) 0.5809(2) 0.0574(12) Uani 1 1 d . U . . .
O11 O 0.6568(4) 0.5405(4) 0.3683(2) 0.0672(14) Uani 1 1 d . U . . .
O12 O 0.4519(4) 0.5270(4) 0.3674(2) 0.0607(13) Uani 1 1 d . U . . .
O13 O 0.5742(4) 0.6592(3) 0.4485(2) 0.0521(11) Uani 1 1 d . U . . .
C14 C 0.7130(6) 0.6932(6) 0.5847(4) 0.065(2) Uani 1 1 d . U . . .
H14A H 0.769882 0.674533 0.623160 0.078 Uiso 1 1 calc R . . . .
H14B H 0.692852 0.760877 0.591364 0.078 Uiso 1 1 calc R . . . .
C15 C 0.6666(6) 0.7220(5) 0.4606(4) 0.0623(18) Uani 1 1 d . U . . .
H15A H 0.646366 0.789510 0.467752 0.075 Uiso 1 1 calc R . . . .
H15B H 0.694569 0.721616 0.421220 0.075 Uiso 1 1 calc R . . . .
C16 C 0.7903(6) 0.5838(5) 0.5119(4) 0.0639(18) Uani 1 1 d . U . . .
H16A H 0.817686 0.582252 0.472301 0.077 Uiso 1 1 calc R . . . .
H16B H 0.847471 0.565877 0.550343 0.077 Uiso 1 1 calc R . . . .
C17 C 0.7526(6) 0.6878(5) 0.5215(4) 0.0595(17) Uani 1 1 d . U . . .
C18 C 0.8485(7) 0.7603(7) 0.5330(5) 0.079(2) Uani 1 1 d . U . . .
H18A H 0.824072 0.828183 0.532864 0.095 Uiso 1 1 calc R . . . .
H18B H 0.897674 0.747137 0.576102 0.095 Uiso 1 1 calc R . . . .
O19 O 0.8992(5) 0.7464(5) 0.4811(3) 0.0911(19) Uani 1 1 d . U . . .
C20 C 0.9967(7) 0.7988(8) 0.4924(6) 0.104(3) Uani 1 1 d . U . . .
H20A H 1.035759 0.792469 0.539056 0.125 Uiso 1 1 calc R . . . .
H20B H 0.983168 0.868555 0.482502 0.125 Uiso 1 1 calc R . . . .
C21 C 1.0612(8) 0.7559(8) 0.4472(6) 0.101(3) Uani 1 1 d . U . . .
C22 C 1.1523(12) 0.8195(12) 0.4483(10) 0.188(7) Uani 1 1 d . U . . .
H22A H 1.198334 0.820774 0.493515 0.225 Uiso 1 1 calc R . . . .
H22B H 1.127804 0.886552 0.436540 0.225 Uiso 1 1 calc R . . . .
O23 O 1.2129(8) 0.7851(9) 0.4016(6) 0.163(4) Uani 1 1 d . U . . .
H23 H 1.252961 0.740362 0.419186 0.245 Uiso 1 1 calc GR . . . .
C24 C 0.9887(13) 0.7483(17) 0.3748(8) 0.205(9) Uani 1 1 d . U . . .
H24A H 0.927688 0.707677 0.375495 0.247 Uiso 1 1 calc R . . . .
H24B H 0.963207 0.813937 0.359567 0.247 Uiso 1 1 calc R . . . .
O25 O 1.0398(18) 0.7080(18) 0.3297(8) 0.348(12) Uani 1 1 d . U . . .
H25 H 1.049521 0.648634 0.337328 0.521 Uiso 1 1 calc R . . . .
C26 C 1.0959(11) 0.6532(9) 0.4689(7) 0.126(4) Uani 1 1 d . U . . .
H26A H 1.036039 0.613498 0.473258 0.151 Uiso 1 1 calc R . . . .
H26B H 1.127777 0.621764 0.436436 0.151 Uiso 1 1 calc R . . . .
O27 O 1.1733(9) 0.6630(10) 0.5337(5) 0.181(5) Uani 1 1 d . U . . .
H27 H 1.231933 0.646520 0.529881 0.271 Uiso 1 1 calc GR . . . .
N28 N 0.3574(6) 0.7871(5) 0.2512(3) 0.086(2) Uani 1 1 d D U . . .
C29 C 0.4506(8) 0.7897(8) 0.2212(5) 0.100(3) Uani 1 1 d D U . . .
H29A H 0.470505 0.858353 0.217567 0.120 Uiso 1 1 calc R . . . .
H29B H 0.428735 0.763054 0.175990 0.120 Uiso 1 1 calc R . . . .
C30 C 0.5473(8) 0.7336(10) 0.2592(5) 0.119(4) Uani 1 1 d D U . . .
H30A H 0.569149 0.758022 0.305005 0.142 Uiso 1 1 calc R . . . .
H30B H 0.530018 0.663874 0.260821 0.142 Uiso 1 1 calc R . . . .
C31 C 0.6369(9) 0.7456(11) 0.2261(6) 0.138(5) Uani 1 1 d D U . . .
H31A H 0.614187 0.718340 0.181149 0.166 Uiso 1 1 calc R . . . .
H31B H 0.648555 0.815975 0.221575 0.166 Uiso 1 1 calc R . . . .
C32 C 0.7361(11) 0.7013(14) 0.2587(8) 0.179(7) Uani 1 1 d D U . . .
H32A H 0.770508 0.740528 0.296983 0.269 Uiso 1 1 calc GR . . . .
H32B H 0.780177 0.698102 0.227928 0.269 Uiso 1 1 calc GR . . . .
H32C H 0.724234 0.635647 0.273137 0.269 Uiso 1 1 calc GR . . . .
C33 C 0.3886(9) 0.8277(7) 0.3236(4) 0.099(3) Uani 1 1 d D U . . .
H33A H 0.325757 0.829040 0.340528 0.119 Uiso 1 1 calc R . . . .
H33B H 0.438355 0.781924 0.351405 0.119 Uiso 1 1 calc R . . . .
C34 C 0.4376(12) 0.9300(9) 0.3318(6) 0.137(4) Uani 1 1 d D U . . .
H34A H 0.392005 0.974672 0.300311 0.164 Uiso 1 1 calc R . . . .
H34B H 0.505253 0.927231 0.320437 0.164 Uiso 1 1 calc R . . . .
C35 C 0.4550(12) 0.9721(11) 0.4024(6) 0.147(5) Uani 1 1 d D U . . .
H35A H 0.489531 0.922779 0.434939 0.176 Uiso 1 1 calc R . . . .
H35B H 0.501198 1.029421 0.407270 0.176 Uiso 1 1 calc R . . . .
C36 C 0.3522(13) 1.0018(10) 0.4165(9) 0.174(7) Uani 1 1 d D U . . .
H36A H 0.312340 1.041733 0.380221 0.260 Uiso 1 1 calc GR . . . .
H36B H 0.366134 1.039169 0.457531 0.260 Uiso 1 1 calc GR . . . .
H36C H 0.312313 0.943534 0.420888 0.260 Uiso 1 1 calc GR . . . .
C37 C 0.2729(8) 0.8525(8) 0.2073(5) 0.101(3) Uani 1 1 d D U . . .
H37A H 0.301467 0.918909 0.207572 0.121 Uiso 1 1 calc R . . . .
H37B H 0.258148 0.828122 0.161551 0.121 Uiso 1 1 calc R . . . .
C38 C 0.1714(9) 0.8588(11) 0.2269(7) 0.146(5) Uani 1 1 d D U . . .
H38A H 0.185719 0.879117 0.273545 0.175 Uiso 1 1 calc R . . . .
H38B H 0.139088 0.793643 0.223084 0.175 Uiso 1 1 calc R . . . .
C39 C 0.0944(11) 0.9310(14) 0.1841(8) 0.175(7) Uani 1 1 d D U . . .
H39A H 0.121874 0.998035 0.191069 0.210 Uiso 0.74(5) 1 calc R . . A 1
H39B H 0.082574 0.914614 0.136900 0.210 Uiso 0.74(5) 1 calc R . . A 1
H39C H 0.132282 0.974091 0.160532 0.210 Uiso 0.26(5) 1 calc R . . A 2
H39D H 0.041963 0.894568 0.150769 0.210 Uiso 0.26(5) 1 calc R . . A 2
C40A C -0.007(2) 0.923(4) 0.205(2) 0.224(19) Uani 0.74(5) 1 d D U . A 1
H40A H -0.030348 0.855021 0.200950 0.335 Uiso 0.74(5) 1 calc GR . . A 1
H40B H -0.059596 0.964110 0.177147 0.335 Uiso 0.74(5) 1 calc GR . . A 1
H40C H 0.005171 0.943290 0.251150 0.335 Uiso 0.74(5) 1 calc GR . . A 1
C40B C 0.039(9) 0.993(8) 0.225(3) 0.224(19) Uani 0.26(5) 1 d D U . A 2
H40D H 0.028390 0.953948 0.261820 0.335 Uiso 0.26(5) 1 calc GR . . A 2
H40E H -0.027672 1.014356 0.197532 0.335 Uiso 0.26(5) 1 calc GR . . A 2
H40F H 0.082357 1.049277 0.242290 0.335 Uiso 0.26(5) 1 calc GR . . A 2
C41 C 0.3192(9) 0.6814(7) 0.2533(5) 0.106(3) Uani 1 1 d D U . . .
H41A H 0.374988 0.643110 0.282790 0.127 Uiso 1 1 calc R . . . .
H41B H 0.258775 0.681490 0.272625 0.127 Uiso 1 1 calc R . . . .
C42 C 0.2876(13) 0.6307(9) 0.1856(6) 0.154(5) Uani 1 1 d D U . . .
H42A H 0.225119 0.663065 0.158101 0.184 Uiso 0.817(15) 1 calc R . . B 1
H42B H 0.344311 0.638463 0.163385 0.184 Uiso 0.817(15) 1 calc R . . B 1
H42C H 0.345931 0.590224 0.179615 0.184 Uiso 0.183(15) 1 calc R . . B 2
H42D H 0.272331 0.680224 0.150300 0.184 Uiso 0.183(15) 1 calc R . . B 2
C43A C 0.265(2) 0.5230(11) 0.1903(9) 0.164(7) Uani 0.817(15) 1 d D U . B 1
H43A H 0.207190 0.514589 0.211655 0.197 Uiso 0.817(15) 1 calc R . . B 1
H43B H 0.326916 0.490029 0.217806 0.197 Uiso 0.817(15) 1 calc R . . B 1
C44A C 0.2351(19) 0.4768(14) 0.1213(10) 0.197(8) Uani 0.817(15) 1 d D U . B 1
H44A H 0.220668 0.407567 0.125175 0.296 Uiso 0.817(15) 1 calc R . . B 1
H44B H 0.173074 0.508921 0.094376 0.296 Uiso 0.817(15) 1 calc R . . B 1
H44C H 0.292579 0.484406 0.100516 0.296 Uiso 0.817(15) 1 calc R . . B 1
C43B C 0.190(4) 0.566(4) 0.180(4) 0.164(7) Uani 0.183(15) 1 d D U . B 2
H43C H 0.174209 0.533176 0.136935 0.197 Uiso 0.183(15) 1 calc R . . B 2
H43D H 0.208983 0.514544 0.214301 0.197 Uiso 0.183(15) 1 calc R . . B 2
C44B C 0.092(4) 0.615(6) 0.188(5) 0.197(8) Uani 0.183(15) 1 d D U . B 2
H44D H 0.036965 0.566119 0.183437 0.296 Uiso 0.183(15) 1 calc R . . B 2
H44E H 0.105245 0.645432 0.231145 0.296 Uiso 0.183(15) 1 calc R . . B 2
H44F H 0.070331 0.664140 0.153468 0.296 Uiso 0.183(15) 1 calc R . . B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H40Aa C40Aa H40B 109.5 . . ?
O2 V1 V3 125.41(15) . 3_666 ?
H40Aa C40Aa H40C 109.5 . . ?
H40Ba C40Aa H40C 109.5 . . ?
H40Db C40Bb H40E 109.5 . . ?
H40Db C40Bb H40F 109.5 . . ?
H40Eb C40Bb H40F 109.5 . . ?
O2 V1 V5 81.60(14) . . ?
O2 V1 O7 77.93(15) . . ?
O2 V1 O10 82.07(18) . . ?
V3 V1 V5 66.18(4) 3_666 . ?
O6 V1 O2 89.4(2) . . ?
O6 V1 V3 87.84(16) . 3_666 ?
O6 V1 V5 34.99(16) . . ?
O6 V1 O7 82.48(16) . . ?
O6 V1 O10 159.2(2) . . ?
O6 V1 O12 94.2(2) . 3_666 ?
O7 V1 V3 47.67(3) . 3_666 ?
O7 V1 V5 47.50(3) . . ?
O9 V1 O2 96.3(2) . . ?
C44Bb C43Bb C42 118(3) . . ?
C44Aa C43Aa H43A 109.6 . . ?
C44Aa C43Aa H43B 109.6 . . ?
O9 V1 V3 137.17(19) . 3_666 ?
O9 V1 V5 137.8(2) . . ?
O9 V1 O6 103.3(3) . . ?
O9 V1 O7 172.0(2) . . ?
H43Aa C43Aa H43B 108.1 . . ?
C43Aa C44Aa H44A 109.5 . . ?
H44Aa C44Aa H44B 109.5 . . ?
C43Aa C44Aa H44B 109.5 . . ?
C43Aa C44Aa H44C 109.5 . . ?
H44Ba C44Aa H44C 109.5 . . ?
H44Aa C44Aa H44C 109.5 . . ?
C44Bb C43Bb H43C 107.9 . . ?
H43Cb C43Bb H43D 107.2 . . ?
C44Bb C43Bb H43D 107.9 . . ?
C43Bb C44Bb H44D 109.5 . . ?
H44Db C44Bb H44E 109.5 . . ?
C43Bb C44Bb H44E 109.5 . . ?
H44Db C44Bb H44F 109.5 . . ?
H44Eb C44Bb H44F 109.5 . . ?
C43Bb C44Bb H44F 109.5 . . ?
C40Aa C39 C38 106.6(14) . . ?
C40Bb C39 C38 112(3) . . ?
C40Aa C39 H39A 110.4 . . ?
H39Aa C39 H39B 108.6 . . ?
C40Aa C39 H39B 110.4 . . ?
C40Bb C39 H39C 109.2 . . ?
H39Cb C39 H39D 107.9 . . ?
C40Bb C39 H39D 109.2 . . ?
C43Aa C42 C41 113.1(11) . . ?
C43Aa C42 H42A 109.0 . . ?
H42Aa C42 H42B 107.8 . . ?
C43Aa C42 H42B 109.0 . . ?
C43Bb C42 H42C 109.5 . . ?
C43Bb C42 H42D 109.5 . . ?
H42Cb C42 H42D 108.1 . . ?
O9 V1 O10 96.5(3) . . ?
O9 V1 O12 103.9(2) . 3_666 ?
O10 V1 V3 81.86(14) . 3_666 ?
O10 V1 V5 124.49(15) . . ?
O10 V1 O7 77.25(14) . . ?
O12 V1 O2 158.0(2) 3_666 . ?
O12 V1 V3 33.36(15) 3_666 3_666 ?
O12 V1 V5 88.96(16) 3_666 . ?
O12 V1 O7 81.01(16) 3_666 . ?
O12 V1 O10 87.1(2) 3_666 . ?
V1 O2 V3 109.6(2) . . ?
C16 O2 V1 119.6(4) . . ?
C16 O2 V3 117.9(4) . . ?
V1 V3 V5 65.89(4) 3_666 . ?
O2 V3 V1 124.15(14) . 3_666 ?
O2 V3 V5 81.03(13) . . ?
O2 V3 O7 76.92(13) . . ?
O4 V3 V1 89.15(15) . 3_666 ?
O4 V3 O2 85.6(2) . . ?
O4 V3 V5 33.45(13) . . ?
O4 V3 O7 80.90(13) . . ?
O4 V3 O13 158.08(18) . . ?
O7 V3 V1 47.42(3) . 3_666 ?
O7 V3 V5 47.50(3) . . ?
O11 V3 V1 138.4(2) . 3_666 ?
O11 V3 O2 96.7(3) . . ?
O11 V3 O4 102.4(2) . . ?
O11 V3 V5 135.8(2) . . ?
O11 V3 O7 172.7(2) . . ?
O11 V3 O12 104.1(3) . . ?
O11 V3 O13 97.4(2) . . ?
O12 V3 V1 34.56(14) . 3_666 ?
O12 V3 O2 158.6(2) . . ?
O12 V3 O4 94.3(2) . . ?
O12 V3 V5 87.17(15) . . ?
O12 V3 O7 81.95(15) . . ?
O12 V3 O13 89.7(2) . . ?
O13 V3 V1 81.95(14) . 3_666 ?
O13 V3 O2 82.93(19) . . ?
O13 V3 V5 125.64(13) . . ?
O13 V3 O7 78.33(12) . . ?
V5 O4 V3 112.1(2) . . ?
V3 V5 V1 65.91(4) . . ?
O4 V5 V1 86.89(15) . . ?
O4 V5 V3 34.50(14) . . ?
O4 V5 O6 93.3(2) . . ?
O4 V5 O7 81.85(15) . . ?
O4 V5 O10 90.7(2) . 3_666 ?
O4 V5 O13 158.8(2) . 3_666 ?
O6 V5 V1 33.71(15) . . ?
O6 V5 V3 88.83(15) . . ?
O6 V5 O7 80.84(15) . . ?
O6 V5 O10 156.9(2) . 3_666 ?
O6 V5 O13 85.9(2) . 3_666 ?
O7 V5 V1 47.16(3) . . ?
O7 V5 V3 47.41(3) . . ?
O8 V5 V1 136.7(2) . . ?
O8 V5 V3 138.0(2) . . ?
O8 V5 O4 103.9(2) . . ?
O8 V5 O6 103.1(3) . . ?
O8 V5 O7 172.7(2) . . ?
O8 V5 O10 97.9(3) . 3_666 ?
O8 V5 O13 97.0(2) . 3_666 ?
O10 V5 V1 124.14(14) 3_666 . ?
O10 V5 V3 81.72(14) 3_666 . ?
O10 V5 O7 77.25(14) 3_666 . ?
O10 V5 O13 82.21(19) 3_666 3_666 ?
O13 V5 V1 80.70(14) 3_666 . ?
O13 V5 V3 124.30(13) 3_666 . ?
O13 V5 O7 77.07(13) 3_666 . ?
V1 O6 V5 111.3(2) . . ?
V1 O7 V1 180.00(5) . 3_666 ?
V1 O7 V3 95.09(5) 3_666 3_666 ?
V1 O7 V3 84.91(5) . 3_666 ?
V1 O7 V3 95.09(5) . . ?
V1 O7 V3 84.91(5) 3_666 . ?
V1 O7 V5 94.66(5) . 3_666 ?
V1 O7 V5 94.66(5) 3_666 . ?
V1 O7 V5 85.34(5) . . ?
V1 O7 V5 85.34(5) 3_666 3_666 ?
V3 O7 V3 180.0 . 3_666 ?
V3 O7 V5 94.91(4) 3_666 . ?
V3 O7 V5 85.10(4) 3_666 3_666 ?
V3 O7 V5 85.10(4) . . ?
V3 O7 V5 94.90(4) . 3_666 ?
V5 O7 V5 180.0 3_666 . ?
V5 O10 V1 110.1(2) 3_666 . ?
C14 O10 V1 118.6(5) . . ?
C14 O10 V5 119.2(5) . 3_666 ?
V3 O12 V1 112.1(2) . 3_666 ?
V3 O13 V5 109.2(2) . 3_666 ?
C15 O13 V3 119.1(4) . . ?
C15 O13 V5 117.7(4) . 3_666 ?
O10 C14 H14A 109.2 . . ?
O10 C14 H14B 109.2 . . ?
O10 C14 C17 111.9(6) . . ?
H14A C14 H14B 107.9 . . ?
C17 C14 H14A 109.2 . . ?
C17 C14 H14B 109.2 . . ?
O13 C15 H15A 109.3 . . ?
O13 C15 H15B 109.3 . . ?
O13 C15 C17 111.7(6) . . ?
H15A C15 H15B 107.9 . . ?
C17 C15 H15A 109.3 . . ?
C17 C15 H15B 109.3 . . ?
O2 C16 H16A 109.4 . . ?
O2 C16 H16B 109.4 . . ?
O2 C16 C17 111.2(6) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C14 C17 C15 110.5(6) . . ?
C14 C17 C18 106.0(6) . . ?
C15 C17 C18 109.2(6) . . ?
C16 C17 C14 110.4(6) . . ?
C16 C17 C15 111.6(6) . . ?
C16 C17 C18 109.0(6) . . ?
C17 C18 H18A 110.0 . . ?
C17 C18 H18B 110.0 . . ?
H18A C18 H18B 108.4 . . ?
O19 C18 C17 108.5(7) . . ?
O19 C18 H18A 110.0 . . ?
O19 C18 H18B 110.0 . . ?
C18 O19 C20 112.6(7) . . ?
O19 C20 H20A 109.9 . . ?
O19 C20 H20B 109.9 . . ?
O19 C20 C21 108.8(9) . . ?
H20A C20 H20B 108.3 . . ?
C21 C20 H20A 109.9 . . ?
C21 C20 H20B 109.9 . . ?
C20 C21 C24 108.5(10) . . ?
C22 C21 C20 110.0(11) . . ?
C22 C21 C24 110.4(13) . . ?
C22 C21 C26 110.9(11) . . ?
C26 C21 C20 110.1(9) . . ?
C26 C21 C24 106.9(13) . . ?
C21 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
C21 C22 O23 112.1(13) . . ?
H22A C22 H22B 107.9 . . ?
O23 C22 H22A 109.2 . . ?
O23 C22 H22B 109.2 . . ?
C22 O23 H23 109.5 . . ?
C21 C24 H24A 109.0 . . ?
C21 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
O25 C24 C21 113.0(15) . . ?
O25 C24 H24A 109.0 . . ?
O25 C24 H24B 109.0 . . ?
C24 O25 H25 109.5 . . ?
C21 C26 H26A 110.5 . . ?
C21 C26 H26B 110.5 . . ?
H26A C26 H26B 108.7 . . ?
O27 C26 C21 106.0(11) . . ?
O27 C26 H26A 110.5 . . ?
O27 C26 H26B 110.5 . . ?
C26 O27 H27 109.5 . . ?
C29 N28 C33 110.4(8) . . ?
C29 N28 C37 106.5(6) . . ?
C29 N28 C41 110.0(8) . . ?
C37 N28 C33 109.9(8) . . ?
C41 N28 C33 108.3(6) . . ?
C41 N28 C37 111.7(8) . . ?
N28 C29 H29A 108.4 . . ?
N28 C29 H29B 108.4 . . ?
N28 C29 C30 115.7(7) . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 C29 110.7(8) . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C30 C31 H31A 108.0 . . ?
C30 C31 H31B 108.0 . . ?
H31A C31 H31B 107.2 . . ?
C32 C31 C30 117.3(10) . . ?
C32 C31 H31A 108.0 . . ?
C32 C31 H31B 108.0 . . ?
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 . . ?
N28 C33 H33A 108.4 . . ?
N28 C33 H33B 108.4 . . ?
H33A C33 H33B 107.4 . . ?
C34 C33 N28 115.6(7) . . ?
C34 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
C33 C34 H34A 108.8 . . ?
C33 C34 H34B 108.8 . . ?
C33 C34 C35 113.7(10) . . ?
H34A C34 H34B 107.7 . . ?
C35 C34 H34A 108.8 . . ?
C35 C34 H34B 108.8 . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 C34 111.3(12) . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
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 . . ?
N28 C37 H37A 108.3 . . ?
N28 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C38 C37 N28 115.8(8) . . ?
C38 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
C37 C38 H38A 109.0 . . ?
C37 C38 H38B 109.0 . . ?
C37 C38 C39 112.7(10) . . ?
H38A C38 H38B 107.8 . . ?
C39 C38 H38A 109.0 . . ?
C39 C38 H38B 109.0 . . ?
C38 C39 H39A 110.4 . . ?
C38 C39 H39B 110.4 . . ?
C38 C39 H39C 109.2 . . ?
C38 C39 H39D 109.2 . . ?
N28 C41 H41A 108.7 . . ?
N28 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
C42 C41 N28 114.4(8) . . ?
C39 C40Aa H40A 109.5 . . ?
C39 C40Aa H40B 109.5 . . ?
C42 C41 H41A 108.7 . . ?
C42 C41 H41B 108.7 . . ?
C41 C42 H42A 109.0 . . ?
C41 C42 H42B 109.0 . . ?
C41 C42 H42C 109.5 . . ?
C41 C42 H42D 109.5 . . ?
C41 C42 C43B 111(2) . . ?
C39 C40Aa H40C 109.5 . . ?
C39 C40Bb H40D 109.5 . . ?
C39 C40Bb H40E 109.5 . . ?
C39 C40Bb H40F 109.5 . . ?
C42 C43Aa H43A 109.6 . . ?
C42 C43Aa H43B 109.6 . . ?
C42 C43Aa C44A 110.4(14) . . ?
C42 C43Bb H43C 107.9 . . ?
C42 C43Bb H43D 107.9 . . ?
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
V1 O2 1.999(5) . ?
V1 V3 3.0187(19) 3_666 ?
V1 V5 3.0333(18) . ?
V1 O6 1.807(5) . ?
V1 O7 2.2315(13) . ?
V1 O9 1.596(5) . ?
V1 O10 2.014(5) . ?
V1 O12 1.848(5) 3_666 ?
C40Aa H40A 0.9600 . ?
C40Aa H40B 0.9600 . ?
C40Aa H40C 0.9600 . ?
C40Bb H40D 0.9600 . ?
C40Bb H40E 0.9600 . ?
C40Bb H40F 0.9600 . ?
C43Aa H43A 0.9700 . ?
C43Aa H43B 0.9700 . ?
C43Aa C44A 1.509(16) . ?
C44Aa H44A 0.9600 . ?
C44Aa H44B 0.9600 . ?
C44Aa H44C 0.9600 . ?
C43Bb H43C 0.9700 . ?
C43Bb H43D 0.9700 . ?
C43Bb C44B 1.48(2) . ?
C44Bb H44D 0.9600 . ?
C44Bb H44E 0.9600 . ?
C44Bb H44F 0.9600 . ?
O2 V3 2.039(5) . ?
O2 C16 1.441(9) . ?
V3 V1 3.0187(19) 3_666 ?
V3 O4 1.853(5) . ?
V3 V5 3.0325(17) . ?
V3 O7 2.2406(11) . ?
V3 O11 1.599(5) . ?
V3 O12 1.791(5) . ?
V3 O13 1.997(5) . ?
O4 V5 1.803(4) . ?
V5 O6 1.867(5) . ?
V5 O7 2.2440(12) . ?
V5 O8 1.598(5) . ?
V5 O10 2.000(5) 3_666 ?
V5 O13 2.056(4) 3_666 ?
O7 V1 2.2315(13) 3_666 ?
O7 V3 2.2407(11) 3_666 ?
O7 V5 2.2440(12) 3_666 ?
O10 V5 2.000(5) 3_666 ?
O10 C14 1.434(8) . ?
O12 V1 1.848(5) 3_666 ?
O13 V5 2.055(4) 3_666 ?
O13 C15 1.443(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C17 1.520(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C17 1.526(10) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.516(10) . ?
C17 C18 1.558(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 O19 1.406(10) . ?
O19 C20 1.422(10) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.520(14) . ?
C21 C22 1.462(15) . ?
C21 C24 1.550(18) . ?
C21 C26 1.491(14) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 O23 1.468(16) . ?
O23 H23 0.8200 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 O25 1.39(2) . ?
O25 H25 0.8200 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 O27 1.459(15) . ?
O27 H27 0.8200 . ?
N28 C29 1.499(10) . ?
N28 C33 1.543(10) . ?
N28 C37 1.518(10) . ?
N28 C41 1.515(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.508(11) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.505(12) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.428(12) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.513(12) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.524(12) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.497(14) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.482(12) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.512(13) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C39 H39D 0.9700 . ?
C39 C40A 1.494(17) . ?
C39 C40B 1.49(2) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.513(12) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
C42 H42D 0.9700 . ?
C42 C43A 1.491(14) . ?
C42 C43B 1.52(2) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.766(4)
2 0.234(4)
