# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_hl394neu
_database_code_depnum_ccdc_archive 'CCDC 2088762'
loop_
_audit_author_name
_audit_author_address
'Christian Nather'
;Institute of Inorganic Chemistry University of Kiel
Germany
;
_audit_update_record             
;
2021-06-08 deposited with the CCDC.	2021-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H48 N12 O78 Sb8 V30'
_chemical_formula_weight         3966.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
H H 0.0000 0.0000 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   16.2776(7)
_cell_length_b                   16.2776(7)
_cell_length_c                   17.7520(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4703.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14821
_cell_measurement_theta_min      2.503
_cell_measurement_theta_max      27.992

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.801
_exptl_crystal_F_000             3708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    5.177
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4385
_exptl_absorpt_correction_T_max  0.4809
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14821
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.503
_diffrn_reflns_theta_max         27.992
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2925
_reflns_number_gt                2229
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'X-AREA (STOE, 2008)'
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0666P)²+0.1449P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2925
_refine_ls_number_parameters     161
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1072
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Sb1 Sb 0.22810(2) 0.84081(2) 0.31981(2) 0.01620(14) Uani 1 1 d . . . . .
V1 V 0.000000 1.000000 0.16776(11) 0.0172(4) Uani 1 4 d S T P . .
V2 V 0.16035(6) 1.02950(6) 0.23097(6) 0.0166(2) Uani 1 1 d . . . . .
V3 V 0.28577(6) 1.04821(6) 0.34913(6) 0.0140(2) Uani 1 1 d . . . . .
V4 V 0.35631(8) 1.05894(8) 0.500000 0.0154(3) Uani 1 2 d S T P . .
V5 V 0.20422(8) 1.14286(8) 0.500000 0.0172(3) Uani 1 2 d S T P . .
V6 V 0.30358(8) 0.88980(8) 0.500000 0.0152(3) Uani 1 2 d S T P . .
O1 O 0.000000 1.000000 0.0772(6) 0.043(3) Uani 1 4 d S T P . .
O2 O 0.0908(2) 0.9369(2) 0.2082(2) 0.0186(8) Uani 1 1 d . . . . .
O3 O 0.2207(3) 1.0400(3) 0.1595(3) 0.0289(10) Uani 1 1 d . . . . .
O4 O 0.2157(3) 0.9604(2) 0.3076(2) 0.0202(9) Uani 1 1 d . . . . .
O5 O 0.3643(3) 1.0615(3) 0.2945(3) 0.0239(9) Uani 1 1 d . . . . .
O6 O 0.2951(2) 1.1275(2) 0.4296(2) 0.0165(8) Uani 1 1 d . . . . .
O7 O 0.1586(4) 1.0553(4) 0.500000 0.0356(17) Uani 1 2 d S T P . .
O8 O 0.4529(4) 1.0833(4) 0.500000 0.0293(15) Uani 1 2 d S T P . .
O9 O 0.3298(2) 0.9743(2) 0.4260(2) 0.0174(8) Uani 1 1 d . . . . .
O10 O 0.2200(3) 0.8472(3) 0.5702(3) 0.0244(10) Uani 1 1 d . . . . .
O11 O 0.3789(4) 0.8260(4) 0.500000 0.0261(14) Uani 1 2 d S T P . .
O12 O 0.1126(2) 0.8091(2) 0.3075(2) 0.0187(8) Uani 1 1 d . . . . .
N1 N 0.5268(4) 1.1093(4) 0.6383(4) 0.0318(13) Uani 1 1 d . . . . .
H1A H 0.568156 1.074747 0.627071 0.048 Uiso 1 1 d R U . . .
H1B H 0.512935 1.104907 0.589351 0.048 Uiso 1 1 d R U . . .
H1C H 0.495935 1.080277 0.670821 0.048 Uiso 1 1 d R U . . .
H1D H 0.551235 1.156667 0.651841 0.048 Uiso 1 1 d R U . . .
N2 N 0.3424(8) 1.2671(8) 0.3523(10) 0.048(4) Uani 0.5 1 d . . P . .


_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
Sb1 O10 1.959(5) 10_556 ?
Sb1 O12 1.961(4) . ?
Sb1 O4 1.970(4) . ?
V1 O1 1.608(10) . ?
V1 O2 1.938(4) . ?
V1 O2 1.938(4) 3_665 ?
V1 O2 1.938(4) 4_465 ?
V1 O2 1.938(4) 2_575 ?
V1 V2 2.8813(12) . ?
V1 V2 2.8813(12) 3_665 ?
V1 V2 2.8813(12) 2_575 ?
V1 V2 2.8813(12) 4_465 ?
V2 O3 1.614(5) . ?
V2 O2 1.914(4) 3_665 ?
V2 O2 1.928(4) . ?
V2 O12 1.981(4) 3_665 ?
V2 O4 1.982(4) . ?
V2 V3 2.9429(14) . ?
V3 O5 1.619(4) . ?
V3 O6 1.931(4) . ?
V3 O9 1.955(4) . ?
V3 O4 1.971(4) . ?
V3 O12 2.007(4) 3_665 ?
V3 V4 2.9192(11) . ?
V4 O8 1.621(6) . ?
V4 O6 1.950(4) 10_556 ?
V4 O6 1.950(4) . ?
V4 O9 1.952(4) 10_556 ?
V4 O9 1.952(4) . ?
V4 V5 2.8274(19) . ?
V4 V6 2.8839(19) . ?
V5 O7 1.606(7) . ?
V5 O6 1.953(4) 10_556 ?
V5 O6 1.953(4) . ?
V5 O10 1.958(4) 3_665 ?
V5 O10 1.958(4) 12_666 ?
V5 V6 3.0310(19) 3_665 ?
V6 O11 1.607(6) . ?
V6 O9 1.950(4) 10_556 ?
V6 O9 1.950(4) . ?
V6 O10 1.971(4) 10_556 ?
V6 O10 1.971(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
O10 Sb1 O12 93.46(18) 10_556 . ?
O10 Sb1 O4 92.84(19) 10_556 . ?
O12 Sb1 O4 98.64(17) . . ?
O1 V1 O2 111.75(14) . . ?
O1 V1 O2 111.75(14) . 3_665 ?
O2 V1 O2 82.11(10) . 3_665 ?
O1 V1 O2 111.75(14) . 4_465 ?
O2 V1 O2 82.11(10) . 4_465 ?
O2 V1 O2 136.5(3) 3_665 4_465 ?
O1 V1 O2 111.75(14) . 2_575 ?
O2 V1 O2 136.5(3) . 2_575 ?
O2 V1 O2 82.11(10) 3_665 2_575 ?
O2 V1 O2 82.11(10) 4_465 2_575 ?
O1 V1 V2 112.92(4) . . ?
O2 V1 V2 41.68(12) . . ?
O2 V1 V2 41.27(12) 3_665 . ?
O2 V1 V2 117.58(14) 4_465 . ?
O2 V1 V2 117.27(14) 2_575 . ?
O1 V1 V2 112.92(4) . 3_665 ?
O2 V1 V2 117.58(13) . 3_665 ?
O2 V1 V2 41.68(12) 3_665 3_665 ?
O2 V1 V2 117.27(14) 4_465 3_665 ?
O2 V1 V2 41.27(12) 2_575 3_665 ?
V2 V1 V2 81.28(3) . 3_665 ?
O1 V1 V2 112.92(4) . 2_575 ?
O2 V1 V2 117.27(14) . 2_575 ?
O2 V1 V2 117.58(14) 3_665 2_575 ?
O2 V1 V2 41.27(12) 4_465 2_575 ?
O2 V1 V2 41.68(12) 2_575 2_575 ?
V2 V1 V2 134.16(8) . 2_575 ?
V2 V1 V2 81.28(3) 3_665 2_575 ?
O1 V1 V2 112.92(4) . 4_465 ?
O2 V1 V2 41.27(12) . 4_465 ?
O2 V1 V2 117.27(14) 3_665 4_465 ?
O2 V1 V2 41.68(12) 4_465 4_465 ?
O2 V1 V2 117.58(13) 2_575 4_465 ?
V2 V1 V2 81.28(3) . 4_465 ?
V2 V1 V2 134.16(8) 3_665 4_465 ?
V2 V1 V2 81.28(3) 2_575 4_465 ?
O3 V2 O2 106.3(2) . 3_665 ?
O3 V2 O2 106.0(2) . . ?
O2 V2 O2 83.0(2) 3_665 . ?
O3 V2 O12 108.3(2) . 3_665 ?
O2 V2 O12 89.79(18) 3_665 3_665 ?
O2 V2 O12 145.62(19) . 3_665 ?
O3 V2 O4 108.9(2) . . ?
O2 V2 O4 144.74(19) 3_665 . ?
O2 V2 O4 88.12(18) . . ?
O12 V2 O4 78.59(17) 3_665 . ?
O3 V2 V1 105.21(19) . . ?
O2 V2 V1 41.91(12) 3_665 . ?
O2 V2 V1 41.96(12) . . ?
O12 V2 V1 127.49(12) 3_665 . ?
O4 V2 V1 125.79(13) . . ?
O3 V2 V3 97.33(19) . . ?
O2 V2 V3 132.07(14) 3_665 . ?
O2 V2 V3 129.60(14) . . ?
O12 V2 V3 42.79(12) 3_665 . ?
O4 V2 V3 41.74(12) . . ?
V1 V2 V3 157.40(5) . . ?
O5 V3 O6 106.9(2) . . ?
O5 V3 O9 102.2(2) . . ?
O6 V3 O9 82.32(17) . . ?
O5 V3 O4 109.3(2) . . ?
O6 V3 O4 143.77(18) . . ?
O9 V3 O4 91.55(17) . . ?
O5 V3 O12 108.5(2) . 3_665 ?
O6 V3 O12 89.06(17) . 3_665 ?
O9 V3 O12 149.37(18) . 3_665 ?
O4 V3 O12 78.24(17) . 3_665 ?
O5 V3 V4 103.36(17) . . ?
O6 V3 V4 41.45(12) . . ?
O9 V3 V4 41.61(12) . . ?
O4 V3 V4 127.87(13) . . ?
O12 V3 V4 127.51(13) 3_665 . ?
O5 V3 V2 97.73(17) . . ?
O6 V3 V2 130.62(13) . . ?
O9 V3 V2 133.49(13) . . ?
O4 V3 V2 42.03(12) . . ?
O12 V3 V2 42.11(12) 3_665 . ?
V4 V3 V2 158.90(5) . . ?
O8 V4 O6 110.8(2) . 10_556 ?
O8 V4 O6 110.8(2) . . ?
O6 V4 O6 79.8(2) 10_556 . ?
O8 V4 O9 112.7(2) . 10_556 ?
O6 V4 O9 81.92(16) 10_556 10_556 ?
O6 V4 O9 136.32(18) . 10_556 ?
O8 V4 O9 112.7(2) . . ?
O6 V4 O9 136.32(18) 10_556 . ?
O6 V4 O9 81.92(16) . . ?
O9 V4 O9 84.6(2) 10_556 . ?
O8 V4 V5 137.0(3) . . ?
O6 V4 V5 43.63(12) 10_556 . ?
O6 V4 V5 43.63(12) . . ?
O9 V4 V5 98.49(12) 10_556 . ?
O9 V4 V5 98.49(12) . . ?
O8 V4 V6 121.5(3) . . ?
O6 V4 V6 113.24(12) 10_556 . ?
O6 V4 V6 113.24(12) . . ?
O9 V4 V6 42.32(12) 10_556 . ?
O9 V4 V6 42.33(12) . . ?
V5 V4 V6 101.58(6) . . ?
O8 V4 V3 113.33(3) . . ?
O6 V4 V3 114.95(13) 10_556 . ?
O6 V4 V3 40.97(12) . . ?
O9 V4 V3 119.25(13) 10_556 . ?
O9 V4 V3 41.69(12) . . ?
V5 V4 V3 71.61(3) . . ?
V6 V4 V3 79.97(3) . . ?
O8 V4 V3 113.33(3) . 10_556 ?
O6 V4 V3 40.97(12) 10_556 10_556 ?
O6 V4 V3 114.95(13) . 10_556 ?
O9 V4 V3 41.69(12) 10_556 10_556 ?
O9 V4 V3 119.26(13) . 10_556 ?
V5 V4 V3 71.61(3) . 10_556 ?
V6 V4 V3 79.97(3) . 10_556 ?
V3 V4 V3 133.11(6) . 10_556 ?
O7 V5 O6 103.7(2) . 10_556 ?
O7 V5 O6 103.7(2) . . ?
O6 V5 O6 79.6(2) 10_556 . ?
O7 V5 O10 111.8(2) . 3_665 ?
O6 V5 O10 89.91(18) 10_556 3_665 ?
O6 V5 O10 144.46(19) . 3_665 ?
O7 V5 O10 111.8(2) . 12_666 ?
O6 V5 O10 144.46(19) 10_556 12_666 ?
O6 V5 O10 89.91(18) . 12_666 ?
O10 V5 O10 79.1(3) 3_665 12_666 ?
O7 V5 V4 88.6(3) . . ?
O6 V5 V4 43.52(12) 10_556 . ?
O6 V5 V4 43.53(12) . . ?
O10 V5 V4 133.19(14) 3_665 . ?
O10 V5 V4 133.19(14) 12_666 . ?
O7 V5 V6 122.2(3) . 3_665 ?
O6 V5 V6 119.53(13) 10_556 3_665 ?
O6 V5 V6 119.53(13) . 3_665 ?
O10 V5 V6 39.68(13) 3_665 3_665 ?
O10 V5 V6 39.68(13) 12_666 3_665 ?
V4 V5 V6 149.21(6) . 3_665 ?
O11 V6 O9 106.8(2) . 10_556 ?
O11 V6 O9 106.8(2) . . ?
O9 V6 O9 84.7(2) 10_556 . ?
O11 V6 O10 107.4(2) . 10_556 ?
O9 V6 O10 145.6(2) 10_556 10_556 ?
O9 V6 O10 88.45(17) . 10_556 ?
O11 V6 O10 107.4(2) . . ?
O9 V6 O10 88.45(17) 10_556 . ?
O9 V6 O10 145.6(2) . . ?
O10 V6 O10 78.5(3) 10_556 . ?
O11 V6 V4 112.9(2) . . ?
O9 V6 V4 42.37(12) 10_556 . ?
O9 V6 V4 42.37(12) . . ?
O10 V6 V4 122.75(14) 10_556 . ?
O10 V6 V4 122.75(14) . . ?
O11 V6 V5 109.4(2) . 11_466 ?
O9 V6 V5 123.05(13) 10_556 11_466 ?
O9 V6 V5 123.05(13) . 11_466 ?
O10 V6 V5 39.35(13) 10_556 11_466 ?
O10 V6 V5 39.35(13) . 11_466 ?
V4 V6 V5 137.64(6) . 11_466 ?
V2 O2 V2 155.3(3) 4_465 . ?
V2 O2 V1 96.82(18) 4_465 . ?
V2 O2 V1 96.36(18) . . ?
Sb1 O4 V3 128.1(2) . . ?
Sb1 O4 V2 133.0(2) . . ?
V3 O4 V2 96.23(18) . . ?
V3 O6 V4 97.57(18) . . ?
V3 O6 V5 119.9(2) . . ?
V4 O6 V5 92.84(18) . . ?
V6 O9 V4 95.30(19) . . ?
V6 O9 V3 145.5(2) . . ?
V4 O9 V3 96.70(18) . . ?
V5 O10 Sb1 130.9(2) 11_466 10_556 ?
V5 O10 V6 101.0(2) 11_466 . ?
Sb1 O10 V6 127.0(2) 10_556 . ?
Sb1 O12 V2 131.6(2) . 4_465 ?
Sb1 O12 V3 131.5(2) . 4_465 ?
V2 O12 V3 95.10(17) 4_465 4_465 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A O9 0.90 2.07 2.933(7) 160.5 9_676 yes
N1 H1B O8 0.90 1.90 2.766(7) 162.0 . yes
N1 H1B O11 0.90 2.62 3.080(7) 112.4 9_676 yes
N1 H1C O5 0.90 2.25 3.005(7) 141.1 10_556 yes
N1 H1D O3 0.90 2.01 2.801(8) 145.9 8_465 yes

_refine_diff_density_max         2.455
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.201



