# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_dynioda
_database_code_depnum_ccdc_archive 'CCDC 1969716'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Dy2 Ni3 O36, 3(O)'
_chemical_formula_sum            'C24 H36 Dy2 Ni3 O39'
_chemical_formula_weight         1449.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         Dy2Ni3C24H36O36
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.4438(6)
_cell_length_b                   14.4438(6)
_cell_length_c                   15.7220(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2840.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3403
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.4920
_cell_measurement_theta_min      2.5860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.667
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 -4 0 0.0120
-5 4 0 0.0213
1 2 5 0.0479
-1 -2 -5 0.0479
-5 -1 0 0.0305
5 1 0 0.0026
5 -4 5 0.0445
0 1 -1 0.0191
-1 5 0 0.0075

_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.033
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
4.9978 -3.9985 -0.0046 0.0612 0.1509 0.2024
-4.9978 3.9985 0.0046 -0.0612 -0.1509 -0.2024
0.9990 1.9967 4.9918 -0.0472 -0.2065 0.1681
-0.9990 -1.9967 -4.9918 0.0472 0.2065 -0.1681
-4.9979 -0.9938 0.0049 0.1994 -0.0469 -0.2398
4.9979 0.9938 -0.0049 -0.1994 0.0469 0.2398
4.9971 -3.9978 4.9884 0.1477 -0.0276 0.3091
0.0002 0.9983 -0.9987 -0.0694 0.0149 -0.0139
-0.9994 4.9932 0.0006 -0.2312 -0.1175 -0.0091

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9541
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.820
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     26.00  52.00   1.00   22.50    --   -0.39  77.00   0.00   26
  2  ω    -40.00 -14.00   1.00   22.50    --   -0.39  77.00   0.00   26
  3  ω     85.00 111.00   1.00   75.00    --   30.29 178.00  90.00   26
  4  ω     -3.00  69.00   1.00   75.00    --   30.29  57.00 -60.00   72
  5  ω    -98.00   3.00   1.00   75.00    --  -31.07 -57.00  30.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0294983000
_diffrn_orient_matrix_UB_12      -0.0522043000
_diffrn_orient_matrix_UB_13      0.0173270000
_diffrn_orient_matrix_UB_21      0.0134959000
_diffrn_orient_matrix_UB_22      -0.0208287000
_diffrn_orient_matrix_UB_23      -0.0357426000
_diffrn_orient_matrix_UB_31      0.0465198000
_diffrn_orient_matrix_UB_32      0.0074906000
_diffrn_orient_matrix_UB_33      0.0213681000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                941
_reflns_number_total             1230
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0349
_refine_ls_restrained_S_all      1.145
_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)+(0.0573P)²+8.4243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1148
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.125) O3W(0.125)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.666667 0.333333 0.250000 0.01942(18) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.0199(3) Uani 1 4 d S T P . .
O1W O 0.4921(4) 0.3512(4) 0.500000 0.0265(10) Uani 1 2 d S T P . .
H1WA H 0.522644 0.341991 0.546061 0.040 Uiso 0.5 1 d R U P . .
H1WB H 0.530950 0.346222 0.458146 0.040 Uiso 0.5 1 d R U P . .
O3 O 0.76489(19) 0.5298(4) 0.250000 0.0312(10) Uani 1 2 d S T P . .
O1 O 0.6139(3) 0.4185(3) 0.3543(2) 0.0310(7) Uani 1 1 d . . . . .
O2 O 0.6154(3) 0.5614(3) 0.4100(3) 0.0458(10) Uani 1 1 d . . . . .
C1 C 0.6484(4) 0.5171(4) 0.3604(3) 0.0309(10) Uani 1 1 d . . . . .
C2 C 0.7405(6) 0.5898(5) 0.3054(5) 0.065(2) Uani 1 1 d . . . . .
H2A H 0.722636 0.635917 0.273080 0.078 Uiso 1 1 calc R U . . .
H2B H 0.802174 0.634490 0.340557 0.078 Uiso 1 1 calc R U . . .
O2W O 0.772(4) 0.790(4) 0.500000 0.111(13) Uiso 0.25 2 d S . P . .
O3W O 0.860(4) 0.845(4) 0.169(4) 0.096(15) Uiso 0.125 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.0221(2) 0.0221(2) 0.0141(3) 0.000 0.000 0.01103(11)
Ni1 0.0247(6) 0.0245(6) 0.0160(5) 0.000 0.000 0.0163(4)
O1W 0.038(3) 0.030(2) 0.020(2) 0.000 0.000 0.023(2)
O3 0.0362(19) 0.028(2) 0.027(2) 0.000 0.0134(19) 0.0139(12)
O1 0.0386(19) 0.0300(17) 0.0260(16) -0.0003(14) 0.0098(14) 0.0185(16)
O2 0.058(3) 0.034(2) 0.049(2) 0.0047(18) 0.032(2) 0.0254(19)
C1 0.036(3) 0.031(2) 0.028(2) 0.003(2) 0.012(2) 0.019(2)
C2 0.084(5) 0.031(3) 0.078(5) 0.006(3) 0.057(4) 0.028(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
Dy1 O3 2.457(5) 2_655 ?
Dy1 O3 2.457(5) . ?
Dy1 O3 2.457(5) 3_665 ?
Dy1 O1 2.391(3) 2_655 ?
Dy1 O1 2.391(3) 11_655 ?
Dy1 O1 2.391(3) 12 ?
Dy1 O1 2.391(3) 10_665 ?
Dy1 O1 2.391(3) . ?
Dy1 O1 2.391(3) 3_665 ?
Ni1 O1W 2.094(4) . ?
Ni1 O1W 2.094(4) 13_666 ?
Ni1 O2 2.022(3) 16_556 ?
Ni1 O2 2.022(3) . ?
Ni1 O2 2.022(3) 13_666 ?
Ni1 O2 2.022(3) 4_665 ?
O1W H1WA 0.8921 . ?
O1W H1WA 0.9(2) 16_556 ?
O1W H1WB 0.8910 . ?
O1W H1WB 0.9(2) 16_556 ?
O3 C2 1.392(6) . ?
O3 C2 1.392(6) 11_655 ?
O1 C1 1.256(6) . ?
O2 C1 1.245(6) . ?
C1 C2 1.491(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
O3 Dy1 O3 120.0 2_655 . ?
O3 Dy1 O3 120.0 3_665 . ?
O3 Dy1 O3 120.0 3_665 2_655 ?
O1 Dy1 O3 73.98(8) 12 2_655 ?
O1 Dy1 O3 63.56(8) . . ?
O1 Dy1 O3 136.15(9) . 3_665 ?
O1 Dy1 O3 136.15(9) 3_665 2_655 ?
O1 Dy1 O3 136.15(9) 12 . ?
O1 Dy1 O3 63.56(8) 3_665 3_665 ?
O1 Dy1 O3 73.99(8) . 2_655 ?
O1 Dy1 O3 63.56(8) 12 3_665 ?
O1 Dy1 O3 73.99(8) 10_665 . ?
O1 Dy1 O3 136.15(9) 10_665 3_665 ?
O1 Dy1 O3 63.56(8) 11_655 . ?
O1 Dy1 O3 136.15(9) 2_655 . ?
O1 Dy1 O3 73.98(8) 2_655 3_665 ?
O1 Dy1 O3 73.98(8) 11_655 3_665 ?
O1 Dy1 O3 63.56(8) 2_655 2_655 ?
O1 Dy1 O3 136.15(9) 11_655 2_655 ?
O1 Dy1 O3 73.99(8) 3_665 . ?
O1 Dy1 O3 63.56(8) 10_665 2_655 ?
O1 Dy1 O1 147.97(16) 12 . ?
O1 Dy1 O1 78.14(13) 11_655 10_665 ?
O1 Dy1 O1 127.12(16) 2_655 10_665 ?
O1 Dy1 O1 127.12(15) 11_655 . ?
O1 Dy1 O1 147.97(16) 11_655 2_655 ?
O1 Dy1 O1 87.70(18) 12 2_655 ?
O1 Dy1 O1 87.70(18) 3_665 11_655 ?
O1 Dy1 O1 78.14(13) 3_665 . ?
O1 Dy1 O1 78.14(13) 3_665 2_655 ?
O1 Dy1 O1 147.97(16) 3_665 10_665 ?
O1 Dy1 O1 78.14(13) 2_655 . ?
O1 Dy1 O1 127.12(15) 12 3_665 ?
O1 Dy1 O1 78.14(13) 12 10_665 ?
O1 Dy1 O1 78.14(13) 12 11_655 ?
O1 Dy1 O1 87.70(18) 10_665 . ?
O1W Ni1 O1W 180.0 13_666 . ?
O2 Ni1 O1W 86.57(14) 4_665 . ?
O2 Ni1 O1W 86.57(14) 13_666 . ?
O2 Ni1 O1W 93.43(14) 13_666 13_666 ?
O2 Ni1 O1W 86.57(14) 16_556 13_666 ?
O2 Ni1 O1W 93.43(14) . . ?
O2 Ni1 O1W 86.57(14) . 13_666 ?
O2 Ni1 O1W 93.43(14) 4_665 13_666 ?
O2 Ni1 O1W 93.43(14) 16_556 . ?
O2 Ni1 O2 180.0 16_556 4_665 ?
O2 Ni1 O2 180.0 . 13_666 ?
O2 Ni1 O2 88.8(3) 4_665 13_666 ?
O2 Ni1 O2 91.2(3) . 4_665 ?
O2 Ni1 O2 88.8(3) . 16_556 ?
O2 Ni1 O2 91.2(3) 16_556 13_666 ?
Ni1 O1W H1WA 112.1 . . ?
Ni1 O1W H1WA 112(5) . 16_556 ?
Ni1 O1W H1WB 111.7 . . ?
Ni1 O1W H1WB 112(6) . 16_556 ?
H1WA O1W H1WA 108.5 . 16_556 ?
H1WA O1W H1WB 102.0 16_556 16_556 ?
H1WA O1W H1WB 102.0 . . ?
H1WA O1W H1WB 7.9 . 16_556 ?
H1WB O1W H1WA 7.9 . 16_556 ?
H1WB O1W H1WB 95.2 . 16_556 ?
C2 O3 Dy1 122.6(3) 11_655 . ?
C2 O3 Dy1 122.6(3) . . ?
C2 O3 C2 114.8(6) . 11_655 ?
C1 O1 Dy1 126.0(3) . . ?
C1 O2 Ni1 131.1(3) . . ?
O1 C1 C2 117.6(4) . . ?
O2 C1 O1 126.4(4) . . ?
O2 C1 C2 116.0(4) . . ?
O3 C2 C1 109.8(4) . . ?
O3 C2 H2A 109.7 . . ?
O3 C2 H2B 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O3 C2 C1 -0.8(8) . . . . ?
Dy1 O1 C1 O2 173.8(4) . . . . ?
Dy1 O1 C1 C2 -8.5(8) . . . . ?
Ni1 O2 C1 O1 1.1(9) . . . . ?
Ni1 O2 C1 C2 -176.5(5) . . . . ?
O1 C1 C2 O3 5.6(9) . . . . ?
O2 C1 C2 O3 -176.6(5) . . . . ?
C2 O3 C2 C1 179.2(8) 11_655 . . . ?

_shelx_res_file                  
;
TITL dynioda_a.res in P6/mcc
    dynioda.res
    created by SHELXL-2018/3 at 12:24:02 on 12-Mar-2020
REM Old TITL dynioda_d.res in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.081, Rweak 0.000, Alpha 0.072, Orientation as input
REM Formula found by SHELXT: C24 O36 Ni3 Dy2
CELL 0.71073 14.4438 14.4438 15.722 90 90 120
ZERR 2 0.0006 0.0006 0.0006 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Dy Ni O
UNIT 48 72 4 6 78

L.S. 50
PLAN  5
TEMP 25(2)
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
OMIT 0 0 2
OMIT 0 0 4
REM <olex2.extras>
REM <HklSrc "%.\\DyNiODA.hkl">
REM </olex2.extras>

WGHT    0.057300    8.424300
FVAR       0.21168
DY1   3    0.666667    0.333333    0.250000    10.16667    0.02207    0.02207 =
         0.01412    0.00000    0.00000    0.01103
NI1   4    0.500000    0.500000    0.500000    10.25000    0.02474    0.02447 =
         0.01595    0.00000    0.00000    0.01629
O1W   5    0.492100    0.351240    0.500000    10.50000    0.03750    0.03023 =
         0.01956    0.00000    0.00000    0.02267
AFIX   7
H1WA  2    0.522644    0.341991    0.546061    10.50000   -1.50000
H1WB  2    0.530950    0.346222    0.458146    10.50000   -1.50000
AFIX   0
O3    5    0.764892    0.529783    0.250000    10.50000    0.03616    0.02787 =
         0.02678    0.00000    0.01342    0.01393
O1    5    0.613923    0.418460    0.354319    11.00000    0.03860    0.03005 =
         0.02604   -0.00030    0.00979    0.01853
O2    5    0.615417    0.561363    0.410028    11.00000    0.05839    0.03361 =
         0.04857    0.00467    0.03230    0.02543
C1    1    0.648424    0.517074    0.360361    11.00000    0.03579    0.03134 =
         0.02849    0.00307    0.01189    0.01890
C2    1    0.740515    0.589776    0.305383    11.00000    0.08359    0.03128 =
         0.07843    0.00602    0.05743    0.02818
AFIX  23
H2A   2    0.722636    0.635917    0.273080    11.00000   -1.20000
H2B   2    0.802174    0.634490    0.340557    11.00000   -1.20000
AFIX   0

O2W   5    0.772148    0.789715    0.500000    10.12500    0.11097
O3W   5    0.860321    0.845011    0.169401    10.12500    0.09606
HKLF 4




REM  dynioda_a.res in P6/mcc
REM wR2 = 0.1148, GooF = S = 1.145, Restrained GooF = 1.145 for all data
REM R1 = 0.0349 for 941 Fo > 4sig(Fo) and 0.0468 for all 1230 data
REM 62 parameters refined using 0 restraints

END

WGHT      0.0573      8.4290

REM Highest difference peak  1.092,  deepest hole -1.035,  1-sigma level  0.156
Q1    1   0.8029  0.7454  0.5000  10.50000  0.05    1.09
Q2    1   0.7316  0.8105  0.5000  10.50000  0.05    1.05
Q3    1   0.5780  0.5780  0.2500  10.50000  0.05    0.97
Q4    1   0.8700  0.8308  0.2492  11.00000  0.05    0.95
Q5    1   0.7786  0.7790  0.4648  11.00000  0.05    0.84
;
_shelx_res_checksum              91387
_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.839
####################################################################### 
# 
# 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_honioda
_database_code_depnum_ccdc_archive 'CCDC 1969720'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Ho2 Ni3 O36, 3(O)'
_chemical_formula_sum            'C24 H36 Ho2 Ni3 O39'
_chemical_formula_weight         1454.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         Ho2Ni3C24H36O36
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.4055(6)
_cell_length_b                   14.4055(6)
_cell_length_c                   15.7515(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2830.8(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3355
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.7890
_cell_measurement_theta_min      2.5730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.835
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1420
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 3 0 0.0195
5 -3 0 0.0195
0 4 -5 0.0382
2 -5 5 0.0506
-5 1 0 0.0237
5 -1 0 0.0101
1 -4 -5 0.0610
-1 4 5 0.0309
0 -1 0 0.0281
0 1 0 0.0075

_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.034
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
-4.9949 2.9976 -0.0008 -0.0130 -0.0760 0.2354
4.9949 -2.9976 0.0008 0.0130 0.0760 -0.2354
-0.0023 3.9935 -4.9983 -0.0913 -0.2974 -0.0735
2.0001 -4.9928 4.9984 0.0865 0.3224 -0.0216
-4.9934 0.9995 0.0009 0.0865 -0.0220 0.2445
4.9934 -0.9995 -0.0009 -0.0865 0.0220 -0.2445
1.0023 -3.9990 -4.9918 0.2794 -0.0826 -0.0869
-1.0023 3.9990 4.9918 -0.2794 0.0826 0.0869
0.0007 -0.9991 0.0009 0.0497 0.0270 0.0045
-0.0007 0.9991 -0.0009 -0.0497 -0.0270 -0.0045

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8784
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         2.828
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     18.00  43.00   1.00   25.00    --   -0.39  57.00 -30.00   25
  2  ω    -34.00  -6.00   1.00   25.00    --   -0.39  57.00 -30.00   28
  3  ω     57.00 106.00   1.00  100.00    --   30.13 178.00 150.00   49
  4  ω     -1.00  56.00   1.00  100.00    --  -30.91   0.00-180.00   57
  5  ω    -96.00 -21.00   1.00  100.00    --  -30.91   0.00-180.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0273037000
_diffrn_orient_matrix_UB_12      -0.0498316000
_diffrn_orient_matrix_UB_13      -0.0215402000
_diffrn_orient_matrix_UB_21      -0.0009810000
_diffrn_orient_matrix_UB_22      -0.0269665000
_diffrn_orient_matrix_UB_23      0.0379534000
_diffrn_orient_matrix_UB_31      -0.0498763000
_diffrn_orient_matrix_UB_32      -0.0045809000
_diffrn_orient_matrix_UB_33      0.0110615000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                947
_reflns_number_total             1223
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      1.118
_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)+(0.0565P)²+9.6315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1115
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.125) O3W(0.125)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.333333 0.666667 0.750000 0.01987(18) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 1.000000 0.500000 0.0203(3) Uani 1 4 d S T P . .
O3 O 0.23530(19) 0.76470(19) 0.750000 0.0320(10) Uani 1 2 d S T P . .
O1 O 0.3864(3) 0.8040(3) 0.6460(2) 0.0314(7) Uani 1 1 d . . . . .
C1 C 0.3518(4) 0.8680(4) 0.6395(3) 0.0320(10) Uani 1 1 d . . . . .
C2 C 0.2595(6) 0.8488(5) 0.6953(5) 0.066(2) Uani 1 1 d . . . . .
H2A H 0.277987 0.913078 0.727711 0.080 Uiso 1 1 calc R U . . .
H2B H 0.197432 0.832188 0.660607 0.080 Uiso 1 1 calc R U . . .
O1W O 0.5078(4) 0.8588(4) 0.500000 0.0284(10) Uani 1 2 d S T P . .
H1WA H 0.478872 0.816187 0.451201 0.043 Uiso 0.5 1 d R U P . .
H1WB H 0.465317 0.808638 0.541741 0.043 Uiso 0.5 1 d R U P . .
O2 O 0.3840(3) 0.9451(3) 0.5895(2) 0.0453(10) Uani 1 1 d . . . . .
O2W O 0.223(4) 1.009(3) 0.500000 0.113(14) Uiso 0.25 2 d S . P . .
O3W O 0.138(4) 0.985(4) 0.833(4) 0.094(15) Uiso 0.125 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ho1 0.0226(2) 0.0226(2) 0.0145(2) 0.000 0.000 0.01128(10)
Ni1 0.0251(6) 0.0169(5) 0.0166(5) 0.000 0.000 0.0087(5)
O3 0.0369(19) 0.0369(19) 0.028(2) 0.0146(18) 0.0146(18) 0.023(2)
O1 0.0401(19) 0.0317(17) 0.0261(15) 0.0098(14) 0.0100(14) 0.0207(15)
C1 0.038(3) 0.028(2) 0.030(2) 0.0088(19) 0.012(2) 0.017(2)
C2 0.083(5) 0.062(4) 0.079(5) 0.051(4) 0.057(4) 0.054(4)
O1W 0.040(3) 0.024(2) 0.022(2) 0.000 0.000 0.017(2)
O2 0.057(3) 0.040(2) 0.048(2) 0.0256(18) 0.0310(19) 0.031(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O3 2.446(5) 3_565 ?
Ho1 O3 2.446(5) 2_665 ?
Ho1 O3 2.446(5) . ?
Ho1 O1 2.382(3) . ?
Ho1 O1 2.381(3) 11_556 ?
Ho1 O1 2.381(3) 10_666 ?
Ho1 O1 2.381(3) 12_566 ?
Ho1 O1 2.381(3) 3_565 ?
Ho1 O1 2.381(3) 2_665 ?
Ni1 O1W 2.093(4) 13_676 ?
Ni1 O1W 2.093(4) . ?
Ni1 O2 2.021(3) 16_556 ?
Ni1 O2 2.021(3) 4_675 ?
Ni1 O2 2.021(3) . ?
Ni1 O2 2.021(3) 13_676 ?
O3 C2 1.382(6) . ?
O3 C2 1.382(6) 10_666 ?
O1 C1 1.252(6) . ?
C1 C2 1.500(7) . ?
C1 O2 1.246(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O1W H1WA 0.9410 . ?
O1W H1WB 0.9417 . ?

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
O3 Ho1 O3 119.999(1) . 2_665 ?
O3 Ho1 O3 119.999(1) . 3_565 ?
O3 Ho1 O3 120.0 3_565 2_665 ?
O1 Ho1 O3 136.02(9) 10_666 3_565 ?
O1 Ho1 O3 63.80(8) . . ?
O1 Ho1 O3 136.02(9) 3_565 . ?
O1 Ho1 O3 136.02(9) 2_665 3_565 ?
O1 Ho1 O3 73.86(8) 10_666 2_665 ?
O1 Ho1 O3 136.02(9) 12_566 . ?
O1 Ho1 O3 63.80(8) 3_565 3_565 ?
O1 Ho1 O3 73.86(8) 2_665 . ?
O1 Ho1 O3 63.80(8) 12_566 2_665 ?
O1 Ho1 O3 136.02(9) . 2_665 ?
O1 Ho1 O3 136.02(9) 11_556 2_665 ?
O1 Ho1 O3 73.86(8) 11_556 . ?
O1 Ho1 O3 73.86(8) 12_566 3_565 ?
O1 Ho1 O3 73.86(8) 3_565 2_665 ?
O1 Ho1 O3 73.86(8) . 3_565 ?
O1 Ho1 O3 63.80(8) 11_556 3_565 ?
O1 Ho1 O3 63.80(8) 2_665 2_665 ?
O1 Ho1 O3 63.80(8) 10_666 . ?
O1 Ho1 O1 77.88(13) 10_666 12_566 ?
O1 Ho1 O1 147.72(16) 10_666 3_565 ?
O1 Ho1 O1 77.88(13) . 3_565 ?
O1 Ho1 O1 87.97(17) 10_666 2_665 ?
O1 Ho1 O1 77.88(13) 2_665 3_565 ?
O1 Ho1 O1 127.60(15) 11_556 3_565 ?
O1 Ho1 O1 127.60(15) 2_665 12_566 ?
O1 Ho1 O1 87.97(17) 12_566 3_565 ?
O1 Ho1 O1 77.88(13) 10_666 11_556 ?
O1 Ho1 O1 87.97(17) 11_556 . ?
O1 Ho1 O1 77.88(13) 11_556 12_566 ?
O1 Ho1 O1 127.60(15) 10_666 . ?
O1 Ho1 O1 77.88(13) 2_665 . ?
O1 Ho1 O1 147.72(16) . 12_566 ?
O1 Ho1 O1 147.72(16) 2_665 11_556 ?
O1W Ni1 O1W 180.0(3) . 13_676 ?
O2 Ni1 O1W 86.83(14) . 13_676 ?
O2 Ni1 O1W 86.83(14) 4_675 . ?
O2 Ni1 O1W 93.17(14) 13_676 13_676 ?
O2 Ni1 O1W 93.17(14) 16_556 . ?
O2 Ni1 O1W 93.17(14) . . ?
O2 Ni1 O1W 86.83(14) 16_556 13_676 ?
O2 Ni1 O1W 93.17(14) 4_675 13_676 ?
O2 Ni1 O1W 86.83(14) 13_676 . ?
O2 Ni1 O2 88.5(3) 4_675 13_676 ?
O2 Ni1 O2 88.5(3) 16_556 . ?
O2 Ni1 O2 91.5(3) 16_556 13_676 ?
O2 Ni1 O2 180.0 13_676 . ?
O2 Ni1 O2 91.5(3) 4_675 . ?
O2 Ni1 O2 180.0 16_556 4_675 ?
C2 O3 Ho1 122.8(3) 10_666 . ?
C2 O3 Ho1 122.8(3) . . ?
C2 O3 C2 114.5(6) . 10_666 ?
C1 O1 Ho1 126.0(3) . . ?
O1 C1 C2 117.3(4) . . ?
O2 C1 O1 126.8(4) . . ?
O2 C1 C2 115.8(4) . . ?
O3 C2 C1 109.8(5) . . ?
O3 C2 H2A 109.7 . . ?
O3 C2 H2B 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
Ni1 O1W H1WA 114.4 . . ?
Ni1 O1W H1WB 114.5 . . ?
H1WA O1W H1WB 99.4 . . ?
C1 O2 Ni1 131.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O3 C2 C1 -0.2(8) . . . . ?
Ho1 O1 C1 C2 -7.7(8) . . . . ?
Ho1 O1 C1 O2 174.4(4) . . . . ?
O1 C1 C2 O3 4.7(9) . . . . ?
O1 C1 O2 Ni1 0.4(9) . . . . ?
C2 O3 C2 C1 179.8(8) 10_666 . . . ?
C2 C1 O2 Ni1 -177.5(5) . . . . ?
O2 C1 C2 O3 -177.2(5) . . . . ?

_shelx_res_file                  
;
TITL honioda_c.res in P6/mcc
    honioda.res
    created by SHELXL-2018/3 at 12:28:18 on 12-Mar-2020
REM Old TITL HoNiODA in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.085, Rweak 0.001, Alpha 0.060, Orientation as input
REM Formula found by SHELXT: C42 O18 Ni3 Ho2
CELL 0.71073 14.4055 14.4055 15.7515 90 90 120
ZERR 2 0.0006 0.0006 0.0006 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Ho Ni O
UNIT 48 72 4 6 78

L.S. 50
PLAN  5
TEMP 25(2)
CONF
BOND $H
LIST 6
fmap 2
acta
MORE -1
OMIT 0 0 2
OMIT 0 0 4
OMIT 2 1 0
REM <olex2.extras>
REM <HklSrc "%.\\HoNiODA.hkl">
REM </olex2.extras>

WGHT    0.056500    9.631500
FVAR       0.21471
HO1   3    0.333333    0.666667    0.750000    10.16667    0.02256    0.02256 =
         0.01449    0.00000    0.00000    0.01128
NI1   4    0.500000    1.000000    0.500000    10.25000    0.02508    0.01689 =
         0.01659    0.00000    0.00000    0.00871
O3    5    0.235297    0.764703    0.750000    10.50000    0.03694    0.03694 =
         0.02775    0.01456    0.01456    0.02271
O1    5    0.386401    0.804021    0.645977    11.00000    0.04008    0.03174 =
         0.02606    0.00975    0.01004    0.02068
C1    1    0.351777    0.867997    0.639478    11.00000    0.03834    0.02818 =
         0.02951    0.00877    0.01156    0.01669
C2    1    0.259477    0.848845    0.695318    11.00000    0.08258    0.06207 =
         0.07917    0.05078    0.05702    0.05445
AFIX  23
H2A   2    0.277987    0.913078    0.727711    11.00000   -1.20000
H2B   2    0.197432    0.832188    0.660607    11.00000   -1.20000
AFIX   0
O1W   5    0.507814    0.858790    0.500000    10.50000    0.03967    0.02436 =
         0.02211    0.00000    0.00000    0.01678
AFIX   7
H1WA  2    0.478872    0.816187    0.451201    10.50000   -1.50000
H1WB  2    0.465317    0.808638    0.541741    10.50000   -1.50000
AFIX   0
O2    5    0.384022    0.945090    0.589507    11.00000    0.05727    0.03989 =
         0.04819    0.02558    0.03103    0.03141

O2W   5    0.223267    1.008986    0.500000    10.12500    0.11263
O3W   5    0.137961    0.984618    0.832518    10.12500    0.09385
HKLF 4




REM  honioda_c.res in P6/mcc
REM wR2 = 0.1115, GooF = S = 1.118, Restrained GooF = 1.118 for all data
REM R1 = 0.0333 for 947 Fo > 4sig(Fo) and 0.0446 for all 1223 data
REM 62 parameters refined using 0 restraints

END

WGHT      0.0562      9.6567

REM Highest difference peak  1.105,  deepest hole -0.709,  1-sigma level  0.147
Q1    1   0.2687  1.0799  0.5000  10.50000  0.05    1.10
Q2    1   0.1949  0.9392  0.5000  10.50000  0.05    0.99
Q3    1   0.2275  1.0063  0.5396  11.00000  0.05    0.88
Q4    1   0.1268  0.9610  0.7494  11.00000  0.05    0.83
Q5    1   0.4187  1.0000  0.7500  10.50000  0.05    0.69
;
_shelx_res_checksum              33213
_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 1.166
_oxdiff_exptl_absorpt_empirical_full_min 0.893
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_smnioda
_database_code_depnum_ccdc_archive 'CCDC 1969718'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Ni3 O36 Sm2, 3(O)'
_chemical_formula_sum            'C24 H36 Ni3 O39 Sm2'
_chemical_formula_weight         1425.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         Sm2Ni3C24H36O36
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'
Ni Ni 0.3393 1.1124 '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'
Sm Sm -0.1638 3.4418 '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      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.7938(11)
_cell_length_b                   14.7938(11)
_cell_length_c                   15.4673(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2931.6(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2725
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.6720
_cell_measurement_theta_min      2.6440
_shelx_estimated_absorpt_T_max   0.899
_shelx_estimated_absorpt_T_min   0.729
_exptl_absorpt_coefficient_mu    3.007
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0255
-1 1 0 0.0101
0 -4 5 0.0462
-1 3 -5 0.0309
4 1 0 0.0335
-5 0 1 0.0059
1 -1 -1 0.0151
-3 6 5 0.0551
2 -7 1 0.0206
-2 7 -1 0.0356

_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.036
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
1.1532 -0.5418 0.0001 -0.0061 -0.0182 0.0519
-1.1532 0.5418 -0.0001 0.0061 0.0182 -0.0519
0.1530 -3.5340 5.0059 -0.0354 -0.2790 -0.1016
-0.6933 2.9216 -5.0056 0.0711 0.2540 0.0676
3.9275 0.7537 -0.0007 -0.1193 0.0387 0.2057
-4.5389 0.4004 1.0012 0.0565 -0.0240 -0.2375
0.6114 -1.1541 -1.0005 0.0629 -0.0147 0.0318
-2.5164 6.3831 5.0024 -0.3501 0.0983 -0.1250
1.9855 -6.9963 1.0034 0.1865 -0.2945 0.0077
-1.9855 6.9963 -1.0034 -0.1865 0.2945 -0.0077

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6642
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.931
_diffrn_reflns_theta_min         2.754
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  41.00   1.00   30.00    --   -0.31 -37.00 120.00   42
  2  ω    -84.00 -51.00   1.00   30.00    --   -0.31 -37.00 120.00   33
  3  ω     -5.00  64.00   1.00  120.00    --   29.03  57.00 150.00   69
  4  ω     60.00 112.00   1.00  120.00    --   29.03 178.00  60.00   52
  5  ω    -89.00 -34.00   1.00  120.00    --  -29.65 178.00 -60.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0231014000
_diffrn_orient_matrix_UB_12      -0.0379633000
_diffrn_orient_matrix_UB_13      -0.0331576000
_diffrn_orient_matrix_UB_21      0.0024157000
_diffrn_orient_matrix_UB_22      0.0386852000
_diffrn_orient_matrix_UB_23      -0.0285036000
_diffrn_orient_matrix_UB_31      0.0502303000
_diffrn_orient_matrix_UB_32      0.0111591000
_diffrn_orient_matrix_UB_33      -0.0139585000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                723
_reflns_number_total             1140
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.058
_refine_diff_density_min         -1.962
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0488
_refine_ls_restrained_S_all      1.035
_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)+(0.1025P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1591
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O1)
3. Rigid body (RIGU) restrains
 O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.16667) O3W(0.08333)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.666667 0.333333 0.250000 0.0192(3) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.0205(4) Uani 1 4 d S T P . .
O1W O 0.4918(5) 0.3549(5) 0.500000 0.0285(15) Uani 1 2 d S T P . .
H1WA H 0.531101 0.333163 0.449956 0.043 Uiso 0.5 1 d R U P . .
H1WB H 0.527756 0.331746 0.551891 0.043 Uiso 0.5 1 d R U P . .
O3 O 0.7636(2) 0.5273(5) 0.250000 0.0293(9) Uani 1 2 d S T P . .
O1 O 0.6151(3) 0.4202(3) 0.3562(3) 0.0293(9) Uani 1 1 d . . . . .
O2 O 0.6128(4) 0.5600(4) 0.4083(3) 0.0462(15) Uani 1 1 d . . . . .
C1 C 0.6481(5) 0.5173(6) 0.3599(5) 0.0321(16) Uani 1 1 d . . . . .
C2 C 0.7375(7) 0.5878(6) 0.3023(7) 0.063(3) Uani 1 1 d . . . . .
H2A H 0.717910 0.629107 0.266552 0.076 Uiso 1 1 calc R U . . .
H2B H 0.797139 0.634985 0.337146 0.076 Uiso 1 1 calc R U . . .
O2W O 0.763(3) 0.783(3) 0.500000 0.112(13) Uiso 0.3333 2 d S . P . .
O3W O 0.916(2) 0.832(5) 0.250000 0.065(15) Uiso 0.1667 2 d S . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm1 0.0212(3) 0.0212(3) 0.0152(4) 0.000 0.000 0.01062(17)
Ni1 0.0239(9) 0.0252(9) 0.0173(7) 0.000 0.000 0.0159(6)
O1W 0.044(4) 0.028(4) 0.025(3) 0.000 0.000 0.026(3)
O3 0.0304(15) 0.029(2) 0.028(2) 0.000 0.0114(15) 0.0147(10)
O1 0.0304(15) 0.029(2) 0.028(2) 0.000 0.0114(15) 0.0147(10)
O2 0.056(4) 0.033(3) 0.048(3) 0.004(3) 0.031(3) 0.021(3)
C1 0.034(4) 0.027(4) 0.036(4) 0.000(3) 0.010(3) 0.016(3)
C2 0.087(7) 0.030(4) 0.072(7) 0.007(4) 0.048(6) 0.030(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
Sm1 O3 2.485(6) 2_655 ?
Sm1 O3 2.485(6) . ?
Sm1 O3 2.485(6) 3_665 ?
Sm1 O1 2.432(4) 11_655 ?
Sm1 O1 2.432(4) 2_655 ?
Sm1 O1 2.432(4) 12 ?
Sm1 O1 2.432(4) 10_665 ?
Sm1 O1 2.432(4) . ?
Sm1 O1 2.432(4) 3_665 ?
Ni1 O1W 2.089(6) . ?
Ni1 O1W 2.089(6) 13_666 ?
Ni1 O2 2.025(5) . ?
Ni1 O2 2.025(5) 16_556 ?
Ni1 O2 2.025(5) 13_666 ?
Ni1 O2 2.025(5) 4_665 ?
O1W H1WA 1.1081 . ?
O1W H1WB 1.1076 . ?
O3 C2 1.397(8) 11_655 ?
O3 C2 1.397(8) . ?
O1 C1 1.266(8) . ?
O2 C1 1.250(8) . ?
C1 C2 1.500(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
O3 Sm1 O3 120.000(1) 3_665 . ?
O3 Sm1 O3 120.0 3_665 2_655 ?
O3 Sm1 O3 120.0 2_655 . ?
O1 Sm1 O3 74.22(10) 12 2_655 ?
O1 Sm1 O3 74.22(10) 11_655 3_665 ?
O1 Sm1 O3 136.86(11) . 3_665 ?
O1 Sm1 O3 136.86(12) 3_665 2_655 ?
O1 Sm1 O3 136.86(12) 12 . ?
O1 Sm1 O3 136.86(12) 10_665 3_665 ?
O1 Sm1 O3 74.22(10) . 2_655 ?
O1 Sm1 O3 62.76(10) 3_665 3_665 ?
O1 Sm1 O3 74.22(10) 10_665 . ?
O1 Sm1 O3 62.76(10) 11_655 . ?
O1 Sm1 O3 136.86(12) 2_655 . ?
O1 Sm1 O3 74.22(10) 2_655 3_665 ?
O1 Sm1 O3 62.76(10) 10_665 2_655 ?
O1 Sm1 O3 62.76(10) . . ?
O1 Sm1 O3 136.86(12) 11_655 2_655 ?
O1 Sm1 O3 62.76(10) 2_655 2_655 ?
O1 Sm1 O3 74.22(10) 3_665 . ?
O1 Sm1 O3 62.76(10) 12 3_665 ?
O1 Sm1 O1 79.39(18) 12 10_665 ?
O1 Sm1 O1 148.4(2) 12 . ?
O1 Sm1 O1 125.5(2) 11_655 . ?
O1 Sm1 O1 125.5(2) 12 3_665 ?
O1 Sm1 O1 79.39(17) 3_665 . ?
O1 Sm1 O1 79.39(17) 2_655 . ?
O1 Sm1 O1 148.4(2) 3_665 10_665 ?
O1 Sm1 O1 86.3(2) 10_665 . ?
O1 Sm1 O1 86.3(2) 12 2_655 ?
O1 Sm1 O1 148.4(2) 2_655 11_655 ?
O1 Sm1 O1 125.5(2) 2_655 10_665 ?
O1 Sm1 O1 79.39(17) 12 11_655 ?
O1 Sm1 O1 86.3(2) 3_665 11_655 ?
O1 Sm1 O1 79.39(17) 11_655 10_665 ?
O1 Sm1 O1 79.39(18) 3_665 2_655 ?
O1W Ni1 O1W 180.0 13_666 . ?
O2 Ni1 O1W 86.4(2) 13_666 . ?
O2 Ni1 O1W 86.4(2) 16_556 13_666 ?
O2 Ni1 O1W 86.4(2) 4_665 . ?
O2 Ni1 O1W 86.4(2) . 13_666 ?
O2 Ni1 O1W 93.6(2) 13_666 13_666 ?
O2 Ni1 O1W 93.6(2) . . ?
O2 Ni1 O1W 93.6(2) 16_556 . ?
O2 Ni1 O1W 93.6(2) 4_665 13_666 ?
O2 Ni1 O2 180.0 16_556 4_665 ?
O2 Ni1 O2 88.9(3) . 16_556 ?
O2 Ni1 O2 91.1(3) . 4_665 ?
O2 Ni1 O2 91.1(3) 16_556 13_666 ?
O2 Ni1 O2 88.9(3) 4_665 13_666 ?
O2 Ni1 O2 180.0 . 13_666 ?
Ni1 O1W H1WA 121.9 . . ?
Ni1 O1W H1WB 121.8 . . ?
H1WA O1W H1WB 90.8 . . ?
C2 O3 Sm1 123.7(4) . . ?
C2 O3 Sm1 123.7(4) 11_655 . ?
C2 O3 C2 112.6(8) 11_655 . ?
C1 O1 Sm1 125.8(4) . . ?
C1 O2 Ni1 131.2(5) . . ?
O1 C1 C2 117.9(6) . . ?
O2 C1 O1 125.3(6) . . ?
O2 C1 C2 116.8(6) . . ?
O3 C2 C1 109.2(6) . . ?
O3 C2 H2A 109.8 . . ?
O3 C2 H2B 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?

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
Sm1 O3 C2 C1 3.3(10) . . . . ?
Sm1 O1 C1 O2 171.5(6) . . . . ?
Sm1 O1 C1 C2 -9.1(10) . . . . ?
Ni1 O2 C1 O1 3.0(12) . . . . ?
Ni1 O2 C1 C2 -176.5(6) . . . . ?
O1 C1 C2 O3 3.3(12) . . . . ?
O2 C1 C2 O3 -177.2(7) . . . . ?
C2 O3 C2 C1 -176.7(10) 11_655 . . . ?

_shelx_res_file                  
;
TITL smnioda.res in P6/mcc
    smnioda.res
    created by SHELXL-2018/3 at 11:58:38 on 12-Mar-2020
REM Old TITL SmNiODA in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.117, Rweak 0.003, Alpha 0.117, Orientation as input
REM Formula found by SHELXT: C48 O12 Ni3 Sm2
CELL 0.71073 14.7938 14.7938 15.4673 90 90 120
ZERR 2 0.0011 0.0011 0.0012 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Ni O Sm
UNIT 48 72 6 78 4
RIGU O3
EADP O3 O1

L.S. 100
PLAN  6
SIZE 0.036 0.06 0.112
TEMP 25(2)
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
OMIT 6 2 1
OMIT 11 4 5
OMIT 13 1 4
OMIT 7 0 0
OMIT 7 0 8
OMIT 7 0 4
OMIT 7 0 12
OMIT 2 1 0
REM <olex2.extras>
REM <HklSrc "%.\\SmNiODA.hkl">
REM </olex2.extras>

WGHT    0.102500
FVAR       0.29319
SM1   5    0.666667    0.333333    0.250000    10.16667    0.02123    0.02123 =
         0.01522    0.00000    0.00000    0.01062
NI1   3    0.500000    0.500000    0.500000    10.25000    0.02392    0.02515 =
         0.01733    0.00000    0.00000    0.01592
O1W   4    0.491765    0.354871    0.500000    10.50000    0.04383    0.02780 =
         0.02520    0.00000    0.00000    0.02638
AFIX   7
H1WA  2    0.531101    0.333163    0.449956    10.50000   -1.50000
H1WB  2    0.527756    0.331746    0.551891    10.50000   -1.50000
AFIX   0
O3    4    0.763647    0.527294    0.250000    10.50000    0.03044    0.02945 =
         0.02771    0.00000    0.01138    0.01473
O1    4    0.615052    0.420219    0.356180    11.00000    0.03044    0.02945 =
         0.02771    0.00000    0.01138    0.01473
O2    4    0.612767    0.560012    0.408316    11.00000    0.05623    0.03263 =
         0.04847    0.00421    0.03141    0.02126
C1    1    0.648082    0.517300    0.359881    11.00000    0.03432    0.02697 =
         0.03589   -0.00043    0.01050    0.01601
C2    1    0.737476    0.587757    0.302307    11.00000    0.08724    0.03034 =
         0.07178    0.00708    0.04825    0.02976
AFIX  23
H2A   2    0.717910    0.629107    0.266552    11.00000   -1.20000
H2B   2    0.797139    0.634985    0.337146    11.00000   -1.20000
AFIX   0

O2W   4    0.762981    0.782973    0.500000    10.16667    0.11243
O3W   4    0.916109    0.832219    0.250000    10.08333    0.06537
HKLF 4




REM  smnioda.res in P6/mcc
REM wR2 = 0.1591, GooF = S = 1.035, Restrained GooF = 1.035 for all data
REM R1 = 0.0488 for 723 Fo > 4sig(Fo) and 0.0736 for all 1140 data
REM 54 parameters refined using 0 restraints

END

WGHT      0.1024      0.0000

REM Highest difference peak  1.058,  deepest hole -1.962,  1-sigma level  0.168
Q1    1   0.7967  0.7462  0.5000  10.50000  0.05    1.06
Q2    1   0.7315  0.8033  0.5000  10.50000  0.05    0.86
Q3    1   0.6435  0.5725  0.2487  11.00000  0.05    0.71
Q4    1   0.5000  0.5000  0.2500  10.25000  0.05    0.65
Q5    1   0.4663  0.3667  0.5000  10.50000  0.05    0.64
Q6    1   0.8889  0.8329  0.1728  11.00000  0.05    0.62
;
_shelx_res_checksum              9414
_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 1.422
_oxdiff_exptl_absorpt_empirical_full_min 0.802
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7008 4316 3065 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.2992 0 3065 nmt -0.5407 0.6129 0.0015 -0.6129 -1.1548 0.0001 0.0009 0.0005
1.0007

_twin_special_details            
;
Component 2 rotated by -147.9196° 
 around [0.00 -0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct)
;
####################################################################### 
# 
# 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_tmnioda
_database_code_depnum_ccdc_archive 'CCDC 1969722'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Ni3 O36 Tm2, 3(O)'
_chemical_formula_sum            'C24 H36 Ni3 O39 Tm2'
_chemical_formula_weight         1462.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         Tm2Ni3C24H36O36
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'
Ni Ni 0.3393 1.1124 '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'
Tm Tm -0.3139 5.2483 '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      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.1712(9)
_cell_length_b                   14.1712(9)
_cell_length_c                   15.9715(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2777.7(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3363
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.1310
_cell_measurement_theta_min      2.5490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.254
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1428
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-9 -11 -5 0.0225
17 -17 3 0.0150
12 7 5 0.0305
-9 20 0 0.0337
-19 13 -5 0.0355
1 0 -5 0.0414
-1 0 5 0.0414
-6 1 1 0.0252
-3 5 3 0.0369

_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.053
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
-8.9309 -10.5639 -4.8850 -0.0082 -0.0034 1.0000
17.2235 -16.9466 3.3954 -0.9237 -0.3829 -0.0089
11.9520 7.2599 5.4271 -0.1622 -0.0672 -0.9845
-9.3768 19.9602 -0.1154 0.7732 0.3205 -0.5473
-19.1638 12.7363 -4.7659 0.8737 0.3622 0.3247
0.9957 -0.0076 -5.0053 -0.0842 0.2135 0.0015
-0.9957 0.0076 5.0053 0.0842 -0.2135 -0.0015
-5.9814 0.9919 0.9955 0.2282 -0.0428 0.2260
-2.9789 4.9869 2.9820 0.2449 -0.0485 -0.1356

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10402
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.275
_diffrn_reflns_theta_min         1.659
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     90.00 119.00   1.00   30.00    --   28.70 178.00   0.00   29
  2  ω    -91.00  -9.00   1.00   30.00    --  -29.48 -57.00-120.00   82
  3  ω    -83.00  58.00   1.00   30.00    --  -29.48   0.00  60.00  141
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0325327000
_diffrn_orient_matrix_UB_12      0.0235115000
_diffrn_orient_matrix_UB_13      0.0103160000
_diffrn_orient_matrix_UB_21      0.0030164000
_diffrn_orient_matrix_UB_22      0.0172314000
_diffrn_orient_matrix_UB_23      -0.0420757000
_diffrn_orient_matrix_UB_31      -0.0476707000
_diffrn_orient_matrix_UB_32      -0.0498685000
_diffrn_orient_matrix_UB_33      -0.0097057000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                937
_reflns_number_total             1203
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1203
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.094
_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)+(0.0614P)²+10.8181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1142
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 H1WA-H1WB
 1.34 with sigma of 0.04
 Ni1-H1WA \\sim Ni1-H1WB
 with sigma of 0.02
3. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.125) O3W(0.125)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.333333 0.666667 0.250000 0.02100(18) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.0203(3) Uani 1 4 d DS T P . .
O3 O 0.5316(4) 0.7658(2) 0.250000 0.0324(11) Uani 1 2 d S T P . .
O1W O 0.3484(4) 0.4941(4) 0.500000 0.0292(10) Uani 1 2 d DS T P . .
H1WA H 0.313(6) 0.436(4) 0.471(5) 0.044 Uiso 0.5 1 d D U P . .
H1WB H 0.364(6) 0.543(5) 0.462(4) 0.044 Uiso 0.5 1 d D U P . .
O1 O 0.4172(3) 0.6127(3) 0.3528(2) 0.0326(8) Uani 1 1 d . . . . .
O2 O 0.5631(3) 0.6185(3) 0.4118(3) 0.0446(10) Uani 1 1 d . . . . .
C1 C 0.5184(4) 0.6499(4) 0.3614(3) 0.0314(10) Uani 1 1 d . . . . .
C2 C 0.5927(5) 0.7445(6) 0.3074(5) 0.068(2) Uani 1 1 d . . . . .
H2A H 0.635274 0.808206 0.342084 0.081 Uiso 1 1 calc R U . . .
H2B H 0.642629 0.728102 0.277869 0.081 Uiso 1 1 calc R U . . .
O2W O 0.791(3) 0.788(3) 0.500000 0.089(11) Uiso 0.25 2 d S . P . .
O3W O 0.867(5) 0.851(5) 0.329(4) 0.101(17) Uiso 0.125 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tm1 0.0238(2) 0.0238(2) 0.0154(3) 0.000 0.000 0.01189(11)
Ni1 0.0245(6) 0.0253(6) 0.0163(5) 0.000 0.000 0.0163(4)
O3 0.029(2) 0.0374(19) 0.028(2) 0.0147(19) 0.000 0.0143(12)
O1W 0.030(2) 0.032(3) 0.028(2) 0.000 0.000 0.017(2)
O1 0.0332(18) 0.0399(19) 0.0260(16) 0.0093(15) 0.0003(14) 0.0193(17)
O2 0.034(2) 0.058(3) 0.045(2) 0.030(2) 0.0044(17) 0.0248(19)
C1 0.034(3) 0.037(3) 0.026(2) 0.010(2) 0.004(2) 0.020(2)
C2 0.037(3) 0.084(5) 0.078(5) 0.060(4) 0.004(3) 0.027(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
Tm1 O3 2.433(5) . ?
Tm1 O3 2.433(5) 3_565 ?
Tm1 O3 2.433(5) 2_665 ?
Tm1 O1 2.368(3) 3_565 ?
Tm1 O1 2.368(3) 12_565 ?
Tm1 O1 2.368(3) 11 ?
Tm1 O1 2.368(3) . ?
Tm1 O1 2.368(3) 10_665 ?
Tm1 O1 2.368(3) 2_665 ?
Ni1 O1W 2.108(5) . ?
Ni1 O1W 2.108(5) 13_666 ?
Ni1 O2 2.026(4) 4_665 ?
Ni1 O2 2.026(4) 16_556 ?
Ni1 O2 2.026(4) . ?
Ni1 O2 2.026(4) 13_666 ?
O3 C2 1.395(6) 12_565 ?
O3 C2 1.395(6) . ?
O1W H1WA 0.85(2) 16_556 ?
O1W H1WA 0.85(2) . ?
O1W H1WB 0.86(2) . ?
O1W H1WB 0.86(2) 16_556 ?
O1 C1 1.263(6) . ?
O2 C1 1.237(6) . ?
C1 C2 1.495(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
O3 Tm1 O3 120.0 . 3_565 ?
O3 Tm1 O3 120.0 2_665 3_565 ?
O3 Tm1 O3 120.0 2_665 . ?
O1 Tm1 O3 135.63(9) 11 . ?
O1 Tm1 O3 64.22(8) 10_665 3_565 ?
O1 Tm1 O3 135.63(9) 10_665 2_665 ?
O1 Tm1 O3 73.75(8) 2_665 . ?
O1 Tm1 O3 73.75(8) 11 3_565 ?
O1 Tm1 O3 64.22(8) 2_665 2_665 ?
O1 Tm1 O3 73.75(8) 10_665 . ?
O1 Tm1 O3 64.22(8) 11 2_665 ?
O1 Tm1 O3 73.75(8) . 3_565 ?
O1 Tm1 O3 135.62(9) . 2_665 ?
O1 Tm1 O3 135.63(9) 12_565 3_565 ?
O1 Tm1 O3 64.22(8) 3_565 3_565 ?
O1 Tm1 O3 73.75(8) 3_565 2_665 ?
O1 Tm1 O3 73.75(8) 12_565 2_665 ?
O1 Tm1 O3 135.63(9) 3_565 . ?
O1 Tm1 O3 64.22(8) 12_565 . ?
O1 Tm1 O3 135.63(9) 2_665 3_565 ?
O1 Tm1 O3 64.22(8) . . ?
O1 Tm1 O1 77.20(14) 11 10_665 ?
O1 Tm1 O1 128.44(16) 12_565 . ?
O1 Tm1 O1 77.20(14) 3_565 . ?
O1 Tm1 O1 77.20(14) 12_565 10_665 ?
O1 Tm1 O1 147.49(17) 12_565 3_565 ?
O1 Tm1 O1 88.75(19) 11 3_565 ?
O1 Tm1 O1 88.75(19) 2_665 12_565 ?
O1 Tm1 O1 147.49(17) 2_665 10_665 ?
O1 Tm1 O1 77.20(14) 2_665 3_565 ?
O1 Tm1 O1 77.19(14) 2_665 . ?
O1 Tm1 O1 128.44(16) 3_565 10_665 ?
O1 Tm1 O1 128.44(16) 11 2_665 ?
O1 Tm1 O1 147.50(17) 11 . ?
O1 Tm1 O1 77.20(14) 11 12_565 ?
O1 Tm1 O1 88.75(18) . 10_665 ?
O1W Ni1 O1W 180.0 13_666 . ?
O2 Ni1 O1W 87.06(14) 13_666 . ?
O2 Ni1 O1W 92.94(14) . . ?
O2 Ni1 O1W 87.06(14) . 13_666 ?
O2 Ni1 O1W 92.94(14) 4_665 13_666 ?
O2 Ni1 O1W 92.94(14) 16_556 . ?
O2 Ni1 O1W 87.06(14) 16_556 13_666 ?
O2 Ni1 O1W 92.94(14) 13_666 13_666 ?
O2 Ni1 O1W 87.06(14) 4_665 . ?
O2 Ni1 O2 88.1(3) 4_665 13_666 ?
O2 Ni1 O2 88.2(3) 16_556 . ?
O2 Ni1 O2 180.0 13_666 . ?
O2 Ni1 O2 91.9(3) 16_556 13_666 ?
O2 Ni1 O2 180.0(2) 16_556 4_665 ?
O2 Ni1 O2 91.8(3) 4_665 . ?
C2 O3 Tm1 122.5(3) 12_565 . ?
C2 O3 Tm1 122.5(3) . . ?
C2 O3 C2 114.9(6) 12_565 . ?
Ni1 O1W H1WA 97(6) . 16_556 ?
Ni1 O1W H1WA 97(6) . . ?
Ni1 O1W H1WB 97(5) . 16_556 ?
Ni1 O1W H1WB 97(5) . . ?
H1WA O1W H1WA 65(10) . 16_556 ?
H1WA O1W H1WB 161(10) . 16_556 ?
H1WA O1W H1WB 100(4) 16_556 16_556 ?
H1WA O1W H1WB 100(4) . . ?
H1WB O1W H1WA 161(10) . 16_556 ?
H1WB O1W H1WB 90(10) . 16_556 ?
C1 O1 Tm1 126.0(3) . . ?
C1 O2 Ni1 131.1(3) . . ?
O1 C1 C2 117.1(4) . . ?
O2 C1 O1 126.8(5) . . ?
O2 C1 C2 116.0(5) . . ?
O3 C2 C1 109.7(5) . . ?
O3 C2 H2A 109.7 . . ?
O3 C2 H2B 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?

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
Tm1 O3 C2 C1 3.9(8) . . . . ?
Tm1 O1 C1 O2 -175.8(4) . . . . ?
Tm1 O1 C1 C2 6.6(8) . . . . ?
Ni1 O2 C1 O1 -0.3(9) . . . . ?
Ni1 O2 C1 C2 177.3(5) . . . . ?
O1 C1 C2 O3 -6.4(9) . . . . ?
O2 C1 C2 O3 175.8(6) . . . . ?
C2 O3 C2 C1 -176.1(8) 12_565 . . . ?

_shelx_res_file                  
;
TITL tmnioda_b.res in P6/mcc
    tmnioda.res
    created by SHELXL-2018/3 at 12:39:34 on 12-Mar-2020
REM Old TITL TmNiODA in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.080, Rweak 0.008, Alpha 0.053, Orientation as input
REM Formula found by SHELXT: C24 O36 Ni3 Tm2
CELL 0.71073 14.1712 14.1712 15.9715 90 90 120
ZERR 2 0.0009 0.0009 0.0017 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Ni O Tm
UNIT 48 72 6 78 4
DFIX 0.85 O1W H1Wa O1W H1Wb
SADI Ni1 H1Wa Ni1 H1Wb
DANG 1.34 H1Wa H1Wb

L.S. 50
PLAN  5
CONF
BOND $H
LIST 6
fmap 2
acta
MORE -1
OMIT 0 0 2
OMIT 2 1 0
OMIT 3 0 0
OMIT 4 0 2
OMIT 1 1 0
OMIT 0 0 4
OMIT 4 1 2
OMIT 2 2 0
REM <olex2.extras>
REM <HklSrc "%.\\TmNiODA.hkl">
REM </olex2.extras>

WGHT    0.061400   10.818101
FVAR       0.22300
TM1   5    0.333333    0.666667    0.250000    10.16667    0.02379    0.02379 =
         0.01542    0.00000    0.00000    0.01189
NI1   3    0.500000    0.500000    0.500000    10.25000    0.02455    0.02526 =
         0.01634    0.00000    0.00000    0.01633
O3    4    0.531585    0.765792    0.250000    10.50000    0.02853    0.03745 =
         0.02819    0.01467    0.00000    0.01427
O1W   4    0.348403    0.494137    0.500000    10.50000    0.03027    0.03151 =
         0.02797    0.00000    0.00000    0.01701
H1WA  2    0.313479    0.436385    0.471494    10.50000   -1.50000
H1WB  2    0.363675    0.542553    0.461830    10.50000   -1.50000
O1    4    0.417242    0.612674    0.352827    11.00000    0.03323    0.03986 =
         0.02604    0.00930    0.00034    0.01930
O2    4    0.563092    0.618510    0.411763    11.00000    0.03379    0.05766 =
         0.04506    0.02968    0.00435    0.02481
C1    1    0.518371    0.649890    0.361368    11.00000    0.03427    0.03699 =
         0.02602    0.00992    0.00374    0.02010
C2    1    0.592730    0.744463    0.307447    11.00000    0.03662    0.08449 =
         0.07826    0.05969    0.00394    0.02718
AFIX  23
H2A   2    0.635274    0.808206    0.342084    11.00000   -1.20000
H2B   2    0.642629    0.728102    0.277869    11.00000   -1.20000
AFIX   0

O2W   4    0.790999    0.788330    0.500000    10.12500    0.08920
O3W   4    0.866839    0.850836    0.329000    10.12500    0.10125
HKLF 4




REM  tmnioda_b.res in P6/mcc
REM wR2 = 0.1142, GooF = S = 1.096, Restrained GooF = 1.094 for all data
REM R1 = 0.0334 for 937 Fo > 4sig(Fo) and 0.0440 for all 1203 data
REM 67 parameters refined using 4 restraints

END

WGHT      0.0612     10.7674

REM Highest difference peak  1.144,  deepest hole -0.484,  1-sigma level  0.164
Q1    1   0.7892  0.7815  0.5401  11.00000  0.05    1.14
Q2    1   0.8110  0.7423  0.5000  10.50000  0.05    1.10
Q3    1   0.8035  0.7604  0.4693  11.00000  0.05    0.99
Q4    1   0.7651  0.8165  0.5000  10.50000  0.05    0.84
Q5    1   0.9206  0.8489  0.3284  11.00000  0.05    0.64
;
_shelx_res_checksum              44537
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.856
####################################################################### 
# 
# 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_ndnioda
_database_code_depnum_ccdc_archive 'CCDC 1969719'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Nd2 Ni3 O36, 3(O)'
_chemical_formula_sum            'C24 H36 Nd2 Ni3 O39'
_chemical_formula_weight         1413.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         Nd2Ni3C24H36O36
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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.9796(11)
_cell_length_b                   14.9796(11)
_cell_length_c                   15.3052(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2974.2(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3568
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.7670
_cell_measurement_theta_min      3.0660
_shelx_estimated_absorpt_T_max   0.915
_shelx_estimated_absorpt_T_min   0.701
_exptl_absorpt_coefficient_mu    2.735
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 5 1 0.0199
-4 -5 -1 0.0199
-5 5 -3 0.0411
5 -5 3 0.0411
-2 5 1 0.0167
2 -5 -1 0.0167
-2 -1 5 0.0527
2 1 -5 0.0527
-5 5 1 0.0187
5 -5 -1 0.0187

_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.033
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
3.9873 4.9908 0.9942 0.0554 0.2773 0.3215
-3.9873 -4.9908 -0.9942 -0.0554 -0.2773 -0.3215
-5.0112 5.0118 -3.0166 -0.0569 -0.2222 0.2041
5.0112 -5.0118 3.0166 0.0569 0.2222 -0.2041
-2.0159 5.0033 0.9936 0.0996 -0.0310 0.2193
2.0159 -5.0033 -0.9936 -0.0996 0.0310 -0.2193
-2.0063 -0.9985 5.0140 0.2300 -0.0689 -0.1314
2.0063 0.9985 -5.0140 -0.2300 0.0689 0.1314
-5.0175 5.0096 0.9933 0.1217 -0.1851 0.1682
5.0175 -5.0096 -0.9933 -0.1217 0.1851 -0.1682

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9422
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.073
_diffrn_reflns_theta_min         3.091
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  12.00   1.00   22.50    --   -0.39 -57.00-120.00   26
  2  ω    -67.00 -34.00   1.00   22.50    --   -0.39 -57.00-120.00   33
  3  ω     57.00 106.00   1.00   75.00    --   30.29 178.00 120.00   49
  4  ω     74.00 100.00   1.00   75.00    --   30.29 178.00 -60.00   26
  5  ω    -26.00  87.00   1.00   75.00    --   30.29 -19.00  60.00  113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0073509000
_diffrn_orient_matrix_UB_12      0.0081021000
_diffrn_orient_matrix_UB_13      0.0445415000
_diffrn_orient_matrix_UB_21      0.0513799000
_diffrn_orient_matrix_UB_22      0.0126553000
_diffrn_orient_matrix_UB_23      0.0093407000
_diffrn_orient_matrix_UB_31      0.0171409000
_diffrn_orient_matrix_UB_32      0.0525032000
_diffrn_orient_matrix_UB_33      -0.0088923000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1084
_reflns_number_total             1434
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      1.097
_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)+(0.0539P)²+7.9290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1101
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O2W(0.16667) O3W(0.08333) H1WA(0.5) H1WB(0.5)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.666667 0.333333 0.250000 0.01848(15) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.0194(2) Uani 1 4 d S T P . .
O1 O 0.6161(2) 0.4222(2) 0.35711(18) 0.0317(6) Uani 1 1 d . . . . .
O3 O 0.76433(14) 0.5287(3) 0.250000 0.0308(8) Uani 1 2 d S T P . .
O2 O 0.6118(3) 0.5597(2) 0.4069(2) 0.0461(8) Uani 1 1 d . . . . .
C1 C 0.6469(3) 0.5169(3) 0.3597(3) 0.0313(8) Uani 1 1 d . . . . .
C2 C 0.7349(4) 0.5866(3) 0.3012(4) 0.0655(19) Uani 1 1 d . . . . .
H2A H 0.714282 0.625408 0.263807 0.079 Uiso 1 1 calc R U . . .
H2B H 0.792885 0.635188 0.336353 0.079 Uiso 1 1 calc R U . . .
O2W O 0.754(3) 0.783(3) 0.500000 0.146(11) Uiso 0.3333 2 d S . P . .
O3W O 0.978(3) 0.830(4) 0.325(3) 0.061(12) Uiso 0.0833 1 d . . P . .
O1W O 0.4910(3) 0.3560(3) 0.500000 0.0259(7) Uani 1 2 d S T P . .
H1WA H 0.521500 0.343300 0.548919 0.039 Uiso 0.5 1 d R U P . .
H1WB H 0.529056 0.347569 0.455219 0.039 Uiso 0.5 1 d R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nd1 0.01994(18) 0.01994(18) 0.0156(2) 0.000 0.000 0.00997(9)
Ni1 0.0221(4) 0.0235(4) 0.0172(4) 0.000 0.000 0.0149(3)
O1 0.0396(15) 0.0276(13) 0.0297(13) 0.0013(11) 0.0138(12) 0.0180(12)
O3 0.0301(14) 0.0247(18) 0.0359(19) 0.000 0.0169(15) 0.0123(9)
O2 0.055(2) 0.0300(15) 0.0557(19) 0.0056(14) 0.0338(16) 0.0230(15)
C1 0.035(2) 0.0267(18) 0.0344(19) 0.0004(16) 0.0127(17) 0.0172(16)
C2 0.081(4) 0.029(2) 0.085(4) 0.006(2) 0.060(3) 0.026(2)
O1W 0.0320(19) 0.0278(18) 0.0225(16) 0.000 0.000 0.0184(16)

_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
Nd1 O1 2.457(3) 3_665 ?
Nd1 O1 2.457(3) 2_655 ?
Nd1 O1 2.457(3) 10_665 ?
Nd1 O1 2.457(3) 11_655 ?
Nd1 O1 2.457(3) 12 ?
Nd1 O1 2.457(3) . ?
Nd1 O3 2.534(4) 3_665 ?
Nd1 O3 2.534(4) . ?
Nd1 O3 2.534(4) 2_655 ?
Ni1 O2 2.033(3) . ?
Ni1 O2 2.034(3) 16_556 ?
Ni1 O2 2.034(3) 4_665 ?
Ni1 O2 2.034(3) 13_666 ?
Ni1 O1W 2.093(4) . ?
Ni1 O1W 2.093(4) 13_666 ?
O1 C1 1.255(4) . ?
O3 C2 1.394(5) . ?
O3 C2 1.394(5) 11_655 ?
O2 C1 1.244(4) . ?
C1 C2 1.501(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O1W H1WA 0.9449 . ?
O1W H1WB 0.9398 . ?

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 Nd1 O1 124.06(12) 3_665 12 ?
O1 Nd1 O1 85.26(14) 12 2_655 ?
O1 Nd1 O1 149.06(13) 3_665 10_665 ?
O1 Nd1 O1 124.06(12) 2_655 10_665 ?
O1 Nd1 O1 149.06(13) 11_655 2_655 ?
O1 Nd1 O1 80.36(10) 2_655 . ?
O1 Nd1 O1 85.26(14) 3_665 11_655 ?
O1 Nd1 O1 80.36(10) 11_655 10_665 ?
O1 Nd1 O1 80.36(10) 3_665 . ?
O1 Nd1 O1 149.06(13) 12 . ?
O1 Nd1 O1 80.36(10) 12 11_655 ?
O1 Nd1 O1 124.06(12) 11_655 . ?
O1 Nd1 O1 80.36(10) 12 10_665 ?
O1 Nd1 O1 80.36(10) 3_665 2_655 ?
O1 Nd1 O1 85.26(14) 10_665 . ?
O1 Nd1 O3 62.03(6) 2_655 2_655 ?
O1 Nd1 O3 74.53(7) 11_655 3_665 ?
O1 Nd1 O3 74.53(7) 2_655 3_665 ?
O1 Nd1 O3 137.37(7) 10_665 3_665 ?
O1 Nd1 O3 137.37(7) 11_655 2_655 ?
O1 Nd1 O3 62.03(6) 11_655 . ?
O1 Nd1 O3 74.53(7) . 2_655 ?
O1 Nd1 O3 137.37(7) . 3_665 ?
O1 Nd1 O3 74.53(7) 12 2_655 ?
O1 Nd1 O3 62.03(6) 12 3_665 ?
O1 Nd1 O3 137.37(7) 12 . ?
O1 Nd1 O3 62.03(6) 10_665 2_655 ?
O1 Nd1 O3 137.37(7) 2_655 . ?
O1 Nd1 O3 74.53(7) 10_665 . ?
O1 Nd1 O3 62.03(6) . . ?
O1 Nd1 O3 137.37(7) 3_665 2_655 ?
O1 Nd1 O3 62.03(6) 3_665 3_665 ?
O1 Nd1 O3 74.53(7) 3_665 . ?
O3 Nd1 O3 120.0 3_665 . ?
O3 Nd1 O3 120.0 3_665 2_655 ?
O3 Nd1 O3 120.0 . 2_655 ?
O2 Ni1 O2 180.00(19) . 13_666 ?
O2 Ni1 O2 180.0 16_556 4_665 ?
O2 Ni1 O2 91.1(2) 16_556 13_666 ?
O2 Ni1 O2 91.1(2) . 4_665 ?
O2 Ni1 O2 88.9(2) . 16_556 ?
O2 Ni1 O2 88.9(2) 4_665 13_666 ?
O2 Ni1 O1W 86.11(11) 16_556 13_666 ?
O2 Ni1 O1W 86.11(11) 4_665 . ?
O2 Ni1 O1W 86.11(11) . 13_666 ?
O2 Ni1 O1W 93.89(11) 4_665 13_666 ?
O2 Ni1 O1W 93.89(11) 16_556 . ?
O2 Ni1 O1W 93.89(11) 13_666 13_666 ?
O2 Ni1 O1W 93.89(11) . . ?
O2 Ni1 O1W 86.11(11) 13_666 . ?
O1W Ni1 O1W 180.0 . 13_666 ?
C1 O1 Nd1 126.5(2) . . ?
C2 O3 Nd1 122.6(2) . . ?
C2 O3 Nd1 122.6(2) 11_655 . ?
C2 O3 C2 114.7(5) . 11_655 ?
C1 O2 Ni1 130.4(3) . . ?
O1 C1 C2 117.8(3) . . ?
O2 C1 O1 126.1(4) . . ?
O2 C1 C2 116.1(3) . . ?
O3 C2 C1 110.1(3) . . ?
O3 C2 H2A 109.6 . . ?
O3 C2 H2B 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
Ni1 O1W H1WA 114.8 . . ?
Ni1 O1W H1WB 114.1 . . ?
H1WA O1W H1WB 99.4 . . ?

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
Nd1 O1 C1 O2 170.4(4) . . . . ?
Nd1 O1 C1 C2 -10.1(6) . . . . ?
Nd1 O3 C2 C1 5.5(6) . . . . ?
Ni1 O2 C1 O1 3.2(8) . . . . ?
Ni1 O2 C1 C2 -176.3(4) . . . . ?
O1 C1 C2 O3 2.4(7) . . . . ?
O2 C1 C2 O3 -178.0(4) . . . . ?
C2 O3 C2 C1 -174.5(6) 11_655 . . . ?

_shelx_res_file                  
;
TITL ndnioda_a.res in P6/mcc
    ndnioda.res
    created by SHELXL-2018/3 at 11:46:55 on 12-Mar-2020
REM Old TITL NdNiODA in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.077, Rweak 0.002, Alpha 0.036, Orientation as input
REM Formula found by SHELXT: C24 O36 Ni3 Nd2
CELL 0.71073 14.9796 14.9796 15.3052 90 90 120
ZERR 2 0.0011 0.0011 0.0012 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Nd Ni O
UNIT 48 72 4 6 78

L.S. 50
PLAN  6
SIZE 0.033 0.057 0.14
TEMP 25(2)
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
OMIT 3 0 0
OMIT 2 2 2
OMIT 3 3 0
OMIT 3 1 2
OMIT 2 1 0
OMIT 4 1 2
OMIT 2 2 0
OMIT 4 0 2
OMIT 1 1 2
REM <olex2.extras>
REM <HklSrc "%.\\NdNiODA.hkl">
REM </olex2.extras>

WGHT    0.053900    7.929000
FVAR       0.29277
ND1   3    0.666667    0.333333    0.250000    10.16667    0.01994    0.01994 =
         0.01556    0.00000    0.00000    0.00997
NI1   4    0.500000    0.500000    0.500000    10.25000    0.02206    0.02349 =
         0.01719    0.00000    0.00000    0.01490
O1    5    0.616140    0.422176    0.357106    11.00000    0.03958    0.02755 =
         0.02970    0.00126    0.01384    0.01798
O3    5    0.764333    0.528665    0.250000    10.50000    0.03012    0.02470 =
         0.03587    0.00000    0.01686    0.01235
O2    5    0.611786    0.559689    0.406940    11.00000    0.05488    0.03004 =
         0.05567    0.00556    0.03376    0.02303
C1    1    0.646937    0.516933    0.359690    11.00000    0.03512    0.02674 =
         0.03444    0.00043    0.01272    0.01719
C2    1    0.734938    0.586606    0.301196    11.00000    0.08101    0.02859 =
         0.08544    0.00616    0.05992    0.02635
AFIX  23
H2A   2    0.714282    0.625408    0.263807    11.00000   -1.20000
H2B   2    0.792885    0.635188    0.336353    11.00000   -1.20000
AFIX   0

O2W   5    0.753556    0.783356    0.500000    10.16667    0.14635
O3W   5    0.977770    0.830113    0.324709    10.08333    0.06109
O1W   5    0.490968    0.355990    0.500000    10.50000    0.03202    0.02783 =
         0.02247    0.00000    0.00000    0.01837
AFIX   7
H1WA  2    0.521500    0.343300    0.548919    10.50000   -1.50000
H1WB  2    0.529056    0.347569    0.455219    10.50000   -1.50000
AFIX   0
HKLF 4




REM  ndnioda_a.res in P6/mcc
REM wR2 = 0.1101, GooF = S = 1.097, Restrained GooF = 1.097 for all data
REM R1 = 0.0308 for 1084 Fo > 4sig(Fo) and 0.0445 for all 1434 data
REM 62 parameters refined using 0 restraints

END

WGHT      0.0539      7.9291

REM Highest difference peak  1.112,  deepest hole -0.521,  1-sigma level  0.130
Q1    1   0.7830  0.7532  0.5000  10.50000  0.05    1.11
Q2    1   0.7200  0.8153  0.5000  10.50000  0.05    0.85
Q3    1   0.7342  0.7900  0.4600  11.00000  0.05    0.71
Q4    1   0.9120  0.8353  0.3232  11.00000  0.05    0.45
Q5    1   0.9127  0.8288  0.3831  11.00000  0.05    0.41
Q6    1   0.9806  0.8377  0.2696  11.00000  0.05    0.41
;
_shelx_res_checksum              48746
_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 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.838
####################################################################### 
# 
# 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_prnioda
_database_code_depnum_ccdc_archive 'CCDC 1969721'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24.001 H36.001 Ni3 O36.001 Pr2, 3(O)'
_chemical_formula_sum            'C24 H36 Ni3 O39 Pr2'
_chemical_formula_weight         1406.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         Pr2Ni3C24H36O36
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'
Ni Ni 0.3393 1.1124 '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'
Pr Pr -0.2180 2.8214 '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      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   15.0750(2)
_cell_length_b                   15.0750(2)
_cell_length_c                   15.2136(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2994.17(9)
_cell_formula_units_Z            1.99992
_cell_measurement_reflns_used    4251
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.7490
_cell_measurement_theta_min      2.6700
_shelx_estimated_absorpt_T_max   0.868
_shelx_estimated_absorpt_T_min   0.745
_exptl_absorpt_coefficient_mu    2.610
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1388
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 0 1 0.0281
5 0 -1 0.0281
-1 5 -1 0.0373
1 -5 1 0.0373
5 -3 0 0.0318
-5 3 0 0.0318
0 0 1 0.0524
0 -1 -5 0.0600
0 5 2 0.0441
5 0 1 0.0307
1 1 -5 0.0606

_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.056
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
-4.9943 0.0001 1.0009 -0.1685 -0.0160 0.2172
4.9943 -0.0001 -1.0009 0.1685 0.0160 -0.2172
-0.9975 4.9922 -0.9986 0.2409 0.0126 0.0761
0.9975 -4.9922 0.9986 -0.2409 -0.0126 -0.0761
4.9934 -2.9953 -0.0020 0.0019 -0.0064 -0.2364
-4.9934 2.9953 0.0020 -0.0019 0.0064 0.2364
-0.0002 0.0002 0.9987 -0.0070 -0.0460 0.0012
0.0009 -0.9995 -4.9937 -0.0184 0.2380 -0.0129
0.0006 4.9929 1.9972 0.2523 -0.1314 0.0366
4.9938 0.0004 0.9966 0.1546 -0.0761 -0.2147
1.0001 0.9975 -4.9942 0.1204 0.2162 -0.0424

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8952
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.702
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     15.00  41.00   1.00   22.50    --   -0.39  77.00  90.00   26
  2  ω    -34.00  -8.00   1.00   22.50    --   -0.39  77.00  90.00   26
  3  ω     15.00  77.00   1.00   60.00    --   30.29  77.00 150.00   62
  4  ω    -62.00  47.00   1.00   60.00    --  -31.07  77.00  60.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0323496000
_diffrn_orient_matrix_UB_12      0.0533142000
_diffrn_orient_matrix_UB_13      -0.0069788000
_diffrn_orient_matrix_UB_21      -0.0060378000
_diffrn_orient_matrix_UB_22      -0.0078906000
_diffrn_orient_matrix_UB_23      -0.0460784000
_diffrn_orient_matrix_UB_31      -0.0432387000
_diffrn_orient_matrix_UB_32      0.0068501000
_diffrn_orient_matrix_UB_33      0.0012051000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1095
_reflns_number_total             1298
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0276
_refine_ls_restrained_S_all      1.065
_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)+(0.0646P)²+6.7181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1091
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.16667) O3W(0.08333)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.666667 0.333333 0.750000 0.01744(16) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 0.000000 0.500000 0.0185(2) Uani 1 4 d S T P . .
O1W O 0.4905(2) 0.1340(2) 0.500000 0.0254(6) Uani 1 2 d S T P . .
H1WA H 0.532275 0.152814 0.454980 0.038 Uiso 0.5 1 d R U P . .
H1WB H 0.524430 0.176911 0.539998 0.038 Uiso 0.5 1 d R U P . .
O1 O 0.6169(2) 0.19361(19) 0.64252(17) 0.0318(5) Uani 1 1 d . . . . .
O3 O 0.76440(13) 0.23560(13) 0.750000 0.0307(8) Uani 1 2 d S T P . .
O2 O 0.6112(2) 0.0515(2) 0.5938(2) 0.0457(7) Uani 1 1 d . . . . .
C1 C 0.6466(3) 0.1293(3) 0.6407(2) 0.0313(7) Uani 1 1 d . . . . .
C2 C 0.7344(4) 0.1482(3) 0.6991(3) 0.0632(16) Uani 1 1 d . . . . .
H2A H 0.714076 0.089515 0.737186 0.076 Uiso 1 1 calc R U . . .
H2B H 0.791580 0.156918 0.663500 0.076 Uiso 1 1 calc R U . . .
O2W O 0.750(3) -0.031(3) 0.500000 0.155(11) Uiso 0.3333 2 d S . P . .
O3W O 0.977(3) 0.150(3) 0.677(3) 0.063(10) Uiso 0.0833 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pr1 0.01874(19) 0.01874(19) 0.0148(2) 0.000 0.000 0.00937(9)
Ni1 0.0210(4) 0.0147(4) 0.0167(4) 0.000 0.000 0.0066(3)
O1W 0.0296(16) 0.0217(15) 0.0233(14) 0.000 0.000 0.0116(13)
O1 0.0402(13) 0.0306(12) 0.0302(11) -0.0129(11) -0.0143(11) 0.0217(11)
O3 0.0291(13) 0.0291(13) 0.0378(18) -0.0167(12) -0.0167(12) 0.0174(15)
O2 0.0558(17) 0.0395(15) 0.0531(16) -0.0290(13) -0.0344(14) 0.0322(14)
C1 0.0349(17) 0.0292(16) 0.0316(16) -0.0112(14) -0.0136(15) 0.0174(14)
C2 0.075(3) 0.055(3) 0.084(4) -0.051(3) -0.057(3) 0.051(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
Pr1 O1 2.468(2) . ?
Pr1 O1 2.468(2) 10_666 ?
Pr1 O1 2.468(2) 12_556 ?
Pr1 O1 2.468(2) 2_655 ?
Pr1 O1 2.468(2) 11_656 ?
Pr1 O1 2.468(2) 3_665 ?
Pr1 O3 2.552(3) . ?
Pr1 O3 2.552(3) 3_665 ?
Pr1 O3 2.552(3) 2_655 ?
Ni1 O1W 2.095(3) 13_656 ?
Ni1 O1W 2.095(3) . ?
Ni1 O2 2.037(2) 16_556 ?
Ni1 O2 2.037(2) 13_656 ?
Ni1 O2 2.037(2) . ?
Ni1 O2 2.037(2) 4_655 ?
O1W H1WA 0.8762 . ?
O1W H1WA 0.88(10) 16_556 ?
O1W H1WB 0.8484 . ?
O1W H1WB 0.85(9) 16_556 ?
O1 C1 1.256(4) . ?
O3 C2 1.395(4) . ?
O3 C2 1.395(4) 10_666 ?
O2 C1 1.242(4) . ?
C1 C2 1.498(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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 Pr1 O1 123.20(11) . 10_666 ?
O1 Pr1 O1 84.71(13) 10_666 2_655 ?
O1 Pr1 O1 149.46(12) . 12_556 ?
O1 Pr1 O1 123.20(11) 2_655 12_556 ?
O1 Pr1 O1 149.46(12) 11_656 2_655 ?
O1 Pr1 O1 80.89(9) 2_655 3_665 ?
O1 Pr1 O1 84.71(13) . 11_656 ?
O1 Pr1 O1 80.89(9) 11_656 12_556 ?
O1 Pr1 O1 80.89(9) . 3_665 ?
O1 Pr1 O1 149.46(12) 10_666 3_665 ?
O1 Pr1 O1 80.89(9) 10_666 11_656 ?
O1 Pr1 O1 123.20(11) 11_656 3_665 ?
O1 Pr1 O1 80.89(9) 10_666 12_556 ?
O1 Pr1 O1 80.89(9) . 2_655 ?
O1 Pr1 O1 84.71(13) 12_556 3_665 ?
O1 Pr1 O3 61.60(6) 12_556 2_655 ?
O1 Pr1 O3 61.60(6) 3_665 3_665 ?
O1 Pr1 O3 74.73(6) 2_655 . ?
O1 Pr1 O3 137.65(6) 12_556 . ?
O1 Pr1 O3 74.73(6) 11_656 . ?
O1 Pr1 O3 74.73(6) . 3_665 ?
O1 Pr1 O3 137.65(6) 2_655 3_665 ?
O1 Pr1 O3 61.60(6) 11_656 3_665 ?
O1 Pr1 O3 137.65(6) 11_656 2_655 ?
O1 Pr1 O3 137.65(6) 3_665 . ?
O1 Pr1 O3 137.65(6) 10_666 3_665 ?
O1 Pr1 O3 74.73(6) 10_666 2_655 ?
O1 Pr1 O3 74.73(6) 12_556 3_665 ?
O1 Pr1 O3 61.60(6) 10_666 . ?
O1 Pr1 O3 137.65(6) . 2_655 ?
O1 Pr1 O3 61.60(6) 2_655 2_655 ?
O1 Pr1 O3 61.60(6) . . ?
O1 Pr1 O3 74.73(6) 3_665 2_655 ?
O3 Pr1 O3 120.0 . 3_665 ?
O3 Pr1 O3 119.997(1) 3_665 2_655 ?
O3 Pr1 O3 120.001(1) . 2_655 ?
O1W Ni1 O1W 180.0 . 13_656 ?
O2 Ni1 O1W 94.15(10) . . ?
O2 Ni1 O1W 85.85(10) 13_656 . ?
O2 Ni1 O1W 85.85(10) 4_655 . ?
O2 Ni1 O1W 85.85(10) 16_556 13_656 ?
O2 Ni1 O1W 94.15(10) 13_656 13_656 ?
O2 Ni1 O1W 85.85(10) . 13_656 ?
O2 Ni1 O1W 94.15(10) 4_655 13_656 ?
O2 Ni1 O1W 94.15(10) 16_556 . ?
O2 Ni1 O2 91.03(19) 4_655 . ?
O2 Ni1 O2 91.03(19) 13_656 16_556 ?
O2 Ni1 O2 180.0 13_656 . ?
O2 Ni1 O2 88.97(19) 13_656 4_655 ?
O2 Ni1 O2 180.00(15) 16_556 4_655 ?
O2 Ni1 O2 88.97(19) 16_556 . ?
Ni1 O1W H1WA 85.8 . . ?
Ni1 O1W H1WA 85.8(5) . 16_556 ?
Ni1 O1W H1WB 115.4 . . ?
Ni1 O1W H1WB 115(3) . 16_556 ?
H1WA O1W H1WA 102.8 . 16_556 ?
H1WA O1W H1WB 104.6 . . ?
H1WA O1W H1WB 104.6 16_556 16_556 ?
H1WA O1W H1WB 29.6 . 16_556 ?
H1WB O1W H1WA 29.6 . 16_556 ?
H1WB O1W H1WB 91.7 . 16_556 ?
C1 O1 Pr1 126.9(2) . . ?
C2 O3 Pr1 122.5(2) . . ?
C2 O3 Pr1 122.5(2) 10_666 . ?
C2 O3 C2 115.0(4) 10_666 . ?
C1 O2 Ni1 130.3(2) . . ?
O1 C1 C2 117.6(3) . . ?
O2 C1 O1 126.2(3) . . ?
O2 C1 C2 116.3(3) . . ?
O3 C2 C1 110.3(3) . . ?
O3 C2 H2A 109.6 . . ?
O3 C2 H2B 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?

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
Pr1 O1 C1 O2 169.8(3) . . . . ?
Pr1 O1 C1 C2 -11.3(6) . . . . ?
Pr1 O3 C2 C1 5.7(5) . . . . ?
Ni1 O2 C1 O1 3.2(7) . . . . ?
Ni1 O2 C1 C2 -175.7(3) . . . . ?
O1 C1 C2 O3 3.0(6) . . . . ?
O2 C1 C2 O3 -178.0(4) . . . . ?
C2 O3 C2 C1 -174.3(5) 10_666 . . . ?

_shelx_res_file                  
;
TITL prnioda_a.res in P6/mcc
    prnioda.res
    created by SHELXL-2018/3 at 11:40:31 on 12-Mar-2020
REM Old TITL prnioda_a.res in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.077, Rweak 0.000, Alpha 0.084, Orientation as input
REM Formula found by SHELXT: C24 O36 Ni3 Pr2
CELL 0.71073 15.075 15.075 15.2136 90 90 120
ZERR 1.99992 0.0002 0.0002 0.0002 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Ni O Pr
UNIT 48 72 6 78 4

L.S. 50
PLAN  6
SIZE 0.056 0.085 0.12
TEMP 25(2)
CONF
BOND $H
list 4
fmap 2
acta
MORE -1
OMIT 0 0 2
OMIT 2 1 0
OMIT 3 1 2
OMIT 4 0 2
OMIT 1 1 0
REM <olex2.extras>
REM <HklSrc "%.\\PrNiODA.hkl">
REM </olex2.extras>

WGHT    0.064600    6.718100
FVAR       0.23448
PR1   5    0.666667    0.333333    0.750000    10.16667    0.01874    0.01874 =
         0.01482    0.00000    0.00000    0.00937
NI1   3    0.500000    0.000000    0.500000    10.25000    0.02101    0.01471 =
         0.01666    0.00000    0.00000    0.00657
O1W   4    0.490483    0.133988    0.500000    10.50000    0.02962    0.02171 =
         0.02333    0.00000    0.00000    0.01164
AFIX   7
H1WA  2    0.532275    0.152814    0.454980    10.50000   -1.50000
H1WB  2    0.524430    0.176911    0.539998    10.50000   -1.50000
AFIX   0
O1    4    0.616868    0.193606    0.642515    11.00000    0.04016    0.03058 =
         0.03018   -0.01287   -0.01427    0.02173
O3    4    0.764395    0.235605    0.750000    10.50000    0.02909    0.02909 =
         0.03785   -0.01670   -0.01670    0.01744
O2    4    0.611204    0.051534    0.593808    11.00000    0.05579    0.03948 =
         0.05310   -0.02898   -0.03442    0.03225
C1    1    0.646647    0.129293    0.640689    11.00000    0.03489    0.02917 =
         0.03162   -0.01123   -0.01362    0.01744
C2    1    0.734366    0.148177    0.699096    11.00000    0.07507    0.05519 =
         0.08389   -0.05115   -0.05739    0.05096
AFIX  23
H2A   2    0.714076    0.089515    0.737186    11.00000   -1.20000
H2B   2    0.791580    0.156918    0.663500    11.00000   -1.20000
AFIX   0

O2W   4    0.750255   -0.031461    0.500000    10.16667    0.15464
O3W   4    0.977024    0.150007    0.676609    10.08333    0.06334
HKLF 4




REM  prnioda_a.res in P6/mcc
REM wR2 = 0.1091, GooF = S = 1.065, Restrained GooF = 1.065 for all data
REM R1 = 0.0276 for 1095 Fo > 4sig(Fo) and 0.0332 for all 1298 data
REM 62 parameters refined using 0 restraints

END

WGHT      0.0644      6.7325

REM Highest difference peak  1.096,  deepest hole -0.460,  1-sigma level  0.127
Q1    1   0.7848  0.0332  0.5000  10.50000  0.05    1.10
Q2    1   0.7210 -0.0889  0.5000  10.50000  0.05    0.84
Q3    1   0.9130  0.0735  0.6688  11.00000  0.05    0.45
Q4    1   0.9942  0.1482  0.7210  11.00000  0.05    0.43
Q5    1   0.9399  0.1172  0.6432  11.00000  0.05    0.42
Q6    1   0.9029  0.0863  0.6161  11.00000  0.05    0.38
;
_shelx_res_checksum              96683
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a mylar loop'
_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 1.061
_oxdiff_exptl_absorpt_empirical_full_min 0.950
####################################################################### 
# 
# 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_ernioda
_database_code_depnum_ccdc_archive 'CCDC 1969717'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
jplatas@ull.edu.es
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Er2 Ni3 O36, 5(O)'
_chemical_formula_sum            'C24 H36 Er2 Ni3 O41'
_chemical_formula_weight         1491.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Er2 Ni3 C24 H36 O41'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.2113(13)
_cell_length_b                   14.2113(13)
_cell_length_c                   15.9401(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2788.0(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2477
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.8110
_cell_measurement_theta_min      2.8500
_shelx_estimated_absorpt_T_max   0.874
_shelx_estimated_absorpt_T_min   0.641
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.0146
3 3 1 0.0278
3 -4 5 0.0168
-3 4 -5 0.0168
-1 6 5 0.0356
1 -6 -5 0.0356
4 -5 0 0.0327
-4 5 0 0.0327

_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.034
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
-0.6164 -0.5383 -0.0000 -0.0444 0.0045 -0.0365
3.0824 2.6913 0.9998 0.1985 -0.0507 0.2080
2.7750 -4.0842 4.9987 -0.0909 -0.2898 -0.0157
-2.7750 4.0842 -4.9987 0.0909 0.2898 0.0157
-0.9213 5.6950 4.9995 -0.0114 -0.0039 0.3779
0.9213 -5.6950 -4.9995 0.0114 0.0039 -0.3779
3.9282 -4.6989 -0.0005 0.0668 -0.1906 -0.1500
-3.9282 4.6989 0.0005 -0.0668 0.1906 0.1500

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8417
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.927
_diffrn_reflns_theta_min         2.867
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     21.00  47.00   1.00   30.00    --   -0.39  77.00 -60.00   26
  2  ω    -37.00 -11.00   1.00   30.00    --   -0.39  77.00 -60.00   26
  3  ω     65.00 102.00   1.00   90.00    --   30.29 178.00-180.00   37
  4  ω     73.00 118.00   1.00   90.00    --   30.29 178.00  90.00   45
  5  ω    -91.00  15.00   1.00   90.00    --  -31.07 -19.00 120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0488187000
_diffrn_orient_matrix_UB_12      0.0265878000
_diffrn_orient_matrix_UB_13      -0.0235615000
_diffrn_orient_matrix_UB_21      -0.0247344000
_diffrn_orient_matrix_UB_22      0.0198880000
_diffrn_orient_matrix_UB_23      -0.0280023000
_diffrn_orient_matrix_UB_31      0.0181539000
_diffrn_orient_matrix_UB_32      0.0471026000
_diffrn_orient_matrix_UB_33      0.0252768000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                769
_reflns_number_total             1310
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      0.913
_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)+(0.0534P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0959
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.25) O3W(0.16667)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.333333 0.666667 0.750000 0.02168(16) Uani 1 6 d S T P . .
Ni1 Ni 0.000000 0.500000 0.500000 0.0220(3) Uani 1 4 d S T P . .
O3 O 0.23447(18) 0.4689(4) 0.750000 0.0328(10) Uani 1 2 d S T P . .
O1W O 0.1442(4) 0.6500(4) 0.500000 0.0286(12) Uani 1 2 d S T P . .
H1WA H 0.187977 0.667460 0.448351 0.043 Uiso 0.5 1 d R U P . .
H1WB H 0.201103 0.662953 0.538992 0.043 Uiso 0.5 1 d R U P . .
O1 O 0.1951(3) 0.5822(3) 0.6474(2) 0.0325(9) Uani 1 1 d . . . . .
C1 C 0.1317(4) 0.4816(4) 0.6391(4) 0.0327(12) Uani 1 1 d . . . . .
C2 C 0.1508(5) 0.4076(5) 0.6937(5) 0.065(2) Uani 1 1 d . . . . .
H2A H 0.084897 0.359621 0.724320 0.078 Uiso 1 1 calc R U . . .
H2B H 0.170037 0.363395 0.659472 0.078 Uiso 1 1 calc R U . . .
O2 O 0.0552(3) 0.4375(3) 0.5887(3) 0.0427(11) Uani 1 1 d . . . . .
O2W O -0.0120(19) 0.2068(19) 0.500000 0.148(9) Uiso 0.5 2 d S . P . .
O3W O 0.123(4) 0.150(4) 0.658(3) 0.142(17) Uiso 0.1667 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Er1 0.02430(18) 0.02430(18) 0.0164(2) 0.000 0.000 0.01215(9)
Ni1 0.0180(5) 0.0258(8) 0.0181(6) 0.000 0.000 0.0080(7)
O3 0.0380(19) 0.029(2) 0.028(2) 0.000 -0.013(3) 0.0144(11)
O1W 0.025(3) 0.027(3) 0.026(3) 0.000 0.000 0.007(2)
O1 0.0323(18) 0.036(2) 0.0269(19) -0.0014(16) -0.0103(15) 0.0148(17)
C1 0.027(3) 0.033(3) 0.034(3) -0.003(3) -0.007(2) 0.012(2)
C2 0.060(4) 0.035(3) 0.080(6) 0.008(4) -0.049(4) 0.009(3)
O2 0.036(2) 0.035(2) 0.045(3) 0.005(2) -0.020(2) 0.0087(18)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O3 2.434(5) 2_665 ?
Er1 O3 2.434(5) . ?
Er1 O3 2.434(4) 3_565 ?
Er1 O1 2.370(3) . ?
Er1 O1 2.370(3) 10_666 ?
Er1 O1 2.370(3) 12_566 ?
Er1 O1 2.370(3) 11_556 ?
Er1 O1 2.370(3) 2_665 ?
Er1 O1 2.370(3) 3_565 ?
Ni1 O1W 2.092(4) . ?
Ni1 O1W 2.092(4) 13_566 ?
Ni1 O2 2.025(4) . ?
Ni1 O2 2.025(4) 16_556 ?
Ni1 O2 2.025(4) 13_566 ?
Ni1 O2 2.025(4) 4_565 ?
O3 C2 1.393(6) 11_556 ?
O3 C2 1.393(7) . ?
O1W H1WA 0.9861 . ?
O1W H1WB 0.9621 . ?
O1 C1 1.259(6) . ?
C1 C2 1.490(8) . ?
C1 O2 1.242(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
O3 Er1 O3 120.000(1) 3_565 . ?
O3 Er1 O3 119.999(1) 3_565 2_665 ?
O3 Er1 O3 120.0 2_665 . ?
O1 Er1 O3 135.89(9) 12_566 2_665 ?
O1 Er1 O3 73.77(8) . 3_565 ?
O1 Er1 O3 135.89(9) 2_665 3_565 ?
O1 Er1 O3 73.77(8) 3_565 2_665 ?
O1 Er1 O3 73.77(8) 12_566 . ?
O1 Er1 O3 135.89(9) 11_556 3_565 ?
O1 Er1 O3 63.99(9) 2_665 2_665 ?
O1 Er1 O3 63.99(8) 3_565 3_565 ?
O1 Er1 O3 63.99(9) 11_556 . ?
O1 Er1 O3 63.99(8) . . ?
O1 Er1 O3 135.89(9) 10_666 . ?
O1 Er1 O3 73.77(8) 10_666 3_565 ?
O1 Er1 O3 73.77(8) 11_556 2_665 ?
O1 Er1 O3 73.77(8) 2_665 . ?
O1 Er1 O3 135.89(9) . 2_665 ?
O1 Er1 O3 63.99(8) 10_666 2_665 ?
O1 Er1 O3 135.89(9) 3_565 . ?
O1 Er1 O3 63.99(8) 12_566 3_565 ?
O1 Er1 O1 77.64(14) 12_566 11_556 ?
O1 Er1 O1 147.55(16) 12_566 2_665 ?
O1 Er1 O1 77.64(14) . 2_665 ?
O1 Er1 O1 127.98(17) 12_566 3_565 ?
O1 Er1 O1 77.64(14) 3_565 2_665 ?
O1 Er1 O1 127.98(17) 10_666 2_665 ?
O1 Er1 O1 147.55(16) 3_565 11_556 ?
O1 Er1 O1 88.22(18) 11_556 2_665 ?
O1 Er1 O1 77.64(14) 12_566 10_666 ?
O1 Er1 O1 147.55(16) 10_666 . ?
O1 Er1 O1 77.64(14) 10_666 11_556 ?
O1 Er1 O1 88.22(18) 12_566 . ?
O1 Er1 O1 77.64(14) 3_565 . ?
O1 Er1 O1 127.98(17) . 11_556 ?
O1 Er1 O1 88.22(18) 3_565 10_666 ?
O1W Ni1 O1W 180.0 13_566 . ?
O2 Ni1 O1W 87.12(15) 13_566 . ?
O2 Ni1 O1W 87.12(15) 16_556 13_566 ?
O2 Ni1 O1W 87.12(15) 4_565 . ?
O2 Ni1 O1W 87.12(15) . 13_566 ?
O2 Ni1 O1W 92.88(15) 13_566 13_566 ?
O2 Ni1 O1W 92.88(15) . . ?
O2 Ni1 O1W 92.88(15) 16_556 . ?
O2 Ni1 O1W 92.88(15) 4_565 13_566 ?
O2 Ni1 O2 180.00(17) 16_556 4_565 ?
O2 Ni1 O2 180.0(2) . 13_566 ?
O2 Ni1 O2 88.6(3) 4_565 13_566 ?
O2 Ni1 O2 88.6(3) . 16_556 ?
O2 Ni1 O2 91.4(3) 16_556 13_566 ?
O2 Ni1 O2 91.4(3) . 4_565 ?
C2 O3 Er1 122.8(3) 11_556 . ?
C2 O3 Er1 122.8(3) . . ?
C2 O3 C2 114.4(6) 11_556 . ?
Ni1 O1W H1WA 115.4 . . ?
Ni1 O1W H1WB 119.8 . . ?
H1WA O1W H1WB 97.3 . . ?
C1 O1 Er1 126.1(3) . . ?
O1 C1 C2 117.5(5) . . ?
O2 C1 O1 126.2(5) . . ?
O2 C1 C2 116.4(5) . . ?
O3 C2 C1 109.5(5) . . ?
O3 C2 H2A 109.8 . . ?
O3 C2 H2B 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C1 O2 Ni1 131.6(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Er1 O3 C2 C1 -2.0(8) . . . . ?
Er1 O1 C1 C2 -5.6(8) . . . . ?
Er1 O1 C1 O2 175.5(5) . . . . ?
O1 C1 C2 O3 4.6(9) . . . . ?
O1 C1 O2 Ni1 1.3(10) . . . . ?
C2 O3 C2 C1 178.0(8) 11_556 . . . ?
C2 C1 O2 Ni1 -177.7(5) . . . . ?
O2 C1 C2 O3 -176.4(5) . . . . ?

_shelx_res_file                  
;
TITL ernioda.res in P6/mcc
    ernioda.res
    created by SHELXL-2018/3 at 12:34:56 on 12-Mar-2020
REM Old TITL ErNiODA in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.126, Rweak 0.002, Alpha 0.089, Orientation as input
REM Formula found by SHELXT: C42 O24 Ni3 Er2
CELL 0.71073 14.21132 14.21132 15.940128 90 90 120
ZERR 2 0.001277 0.001277 0.001781 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Er Ni O
UNIT 48 72 4 6 82

L.S. 50
PLAN  5
SIZE 0.034 0.048 0.12
CONF
BOND $H
LIST 4
MORE -1
fmap 2
acta
OMIT 13 4 7
OMIT 7 4 17
OMIT 13 3 9
OMIT 6 3 18
OMIT 13 1 6
OMIT 2 1 0
OMIT 9 2 13
REM <olex2.extras>
REM <HklSrc "%.\\ErNiODA.hkl">
REM </olex2.extras>

WGHT    0.053400
FVAR       1.13583
ER1   3    0.333333    0.666667    0.750000    10.16667    0.02430    0.02430 =
         0.01643    0.00000    0.00000    0.01215
NI1   4    0.000000    0.500000    0.500000    10.25000    0.01796    0.02584 =
         0.01814    0.00000    0.00000    0.00795
O3    5    0.234469    0.468938    0.750000    10.50000    0.03801    0.02889 =
         0.02833    0.00000   -0.01341    0.01445
O1W   5    0.144185    0.650022    0.500000    10.50000    0.02486    0.02653 =
         0.02620    0.00000    0.00000    0.00667
AFIX   7
H1WA  2    0.187977    0.667460    0.448351    10.50000   -1.50000
H1WB  2    0.201103    0.662953    0.538992    10.50000   -1.50000
AFIX   0
O1    5    0.195083    0.582223    0.647430    11.00000    0.03226    0.03560 =
         0.02690   -0.00144   -0.01026    0.01481
C1    1    0.131748    0.481635    0.639140    11.00000    0.02702    0.03271 =
         0.03440   -0.00313   -0.00750    0.01192
C2    1    0.150770    0.407644    0.693737    11.00000    0.05973    0.03526 =
         0.07963    0.00774   -0.04865    0.00854
AFIX  23
H2A   2    0.084897    0.359621    0.724320    11.00000   -1.20000
H2B   2    0.170037    0.363395    0.659472    11.00000   -1.20000
AFIX   0
O2    5    0.055178    0.437482    0.588688    11.00000    0.03565    0.03522 =
         0.04506    0.00487   -0.02046    0.00868

O2W   5   -0.012028    0.206849    0.500000    10.25000    0.14837
O3W   5    0.122524    0.150102    0.658412    10.16667    0.14230
HKLF 4




REM  ernioda.res in P6/mcc
REM wR2 = 0.0959, GooF = S = 0.913, Restrained GooF = 0.913 for all data
REM R1 = 0.0466 for 769 Fo > 4sig(Fo) and 0.0808 for all 1310 data
REM 62 parameters refined using 0 restraints

END

WGHT      0.0534      0.0000

REM Highest difference peak  0.852,  deepest hole -0.676,  1-sigma level  0.143
Q1    1  -0.0808  0.1775  0.5000  10.50000  0.05    0.85
Q2    1   0.0448  0.2348  0.5000  10.50000  0.05    0.70
Q3    1   0.1158  0.1158  0.7500  10.50000  0.05    0.62
Q4    1  -0.0016  0.2161  0.5525  11.00000  0.05    0.62
Q5    1   0.3333  0.6667  0.8073  10.33333  0.05    0.57
;
_shelx_res_checksum              88734
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.825
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5055 5791 3426 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.4945 0 3426 nmt 0.6161 -0.5389 0.0003 0.5382 1.1546 0.0000 -0.0000 0.0001
0.9995

_twin_special_details            
;
Component 2 rotated by 27.7636° 
 around [0.00 -0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct)
;
####################################################################### 
# 
# 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_tbnioda
_database_code_depnum_ccdc_archive 'CCDC 1969725'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
jplatas@ull.edu.es
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Ni3 O36 Tb2, 5(O)'
_chemical_formula_sum            'C24 H36 Ni3 O41 Tb2'
_chemical_formula_weight         1474.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Tb2 Ni3 C24 H36 O41'
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'
Ni Ni 0.3393 1.1124 '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'
Tb Tb -0.1723 4.1537 '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      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.5537(7)
_cell_length_b                   14.5537(7)
_cell_length_c                   15.6318(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2867.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3373
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.7560
_cell_measurement_theta_min      2.5880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.497
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1444
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 7 0 0.0219
5 -6 0 0.0300
-5 6 0 0.0206
-4 1 -5 0.0764
5 -1 0 0.0246
-5 1 0 0.0246
-3 3 5 0.0755
3 -3 -5 0.0755
2 -7 0 0.0219

_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.044
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
-2.1031 7.0078 0.0629 0.0853 0.3253 0.0993
5.0635 -5.9211 0.0391 -0.2184 -0.2234 0.0165
-5.0635 5.9211 -0.0391 0.2184 0.2234 -0.0165
-3.9289 0.9340 -5.0888 0.2755 -0.0996 0.0853
4.9791 -0.8782 0.1245 -0.2206 0.0330 0.1316
-4.9791 0.8782 -0.1245 0.2206 -0.0330 -0.1316
-3.0857 2.9178 4.9589 0.0323 0.1867 -0.2096
3.0857 -2.9178 -4.9589 -0.0323 -0.1867 0.2096
2.1031 -7.0078 -0.0629 -0.0853 -0.3253 -0.0993

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8199
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.606
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00   4.00   1.00   22.50    --   -0.39 -37.00-180.00   26
  2  ω     24.00  49.00   1.00   22.50    --   -0.39 -37.00-180.00   25
  3  ω     81.00 109.00   1.00   90.00    --   30.29 178.00 120.00   28
  4  ω   -105.00  -1.00   1.00   90.00    --  -31.07 -57.00 120.00  104
  5  ω    -72.00 -28.00   1.00   90.00    --  -31.07 -37.00 -30.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0439525000
_diffrn_orient_matrix_UB_12      -0.0008289000
_diffrn_orient_matrix_UB_13      -0.0203511000
_diffrn_orient_matrix_UB_21      0.0151589000
_diffrn_orient_matrix_UB_22      0.0508111000
_diffrn_orient_matrix_UB_23      0.0171911000
_diffrn_orient_matrix_UB_31      0.0315706000
_diffrn_orient_matrix_UB_32      0.0239768000
_diffrn_orient_matrix_UB_33      -0.0367322000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                992
_reflns_number_total             1245
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.704
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.300
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1057P)²+5.8554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1717
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.16667) O3W(0.25)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.666667 0.333333 0.750000 0.0199(3) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.0201(4) Uani 1 4 d S T P . .
O1W O 0.6477(4) 0.5084(4) 0.500000 0.0291(10) Uani 1 2 d S T P . .
H1WA H 0.657018 0.485926 0.450027 0.044 Uiso 0.5 1 d R U P . .
H1WB H 0.648241 0.460931 0.536304 0.044 Uiso 0.5 1 d R U P . .
O3 O 0.4706(5) 0.2353(2) 0.750000 0.0323(12) Uani 1 2 d S T P . .
O1 O 0.5811(3) 0.3856(3) 0.6452(2) 0.0328(8) Uani 1 1 d . . . . .
O2 O 0.4391(3) 0.3853(3) 0.5906(3) 0.0484(11) Uani 1 1 d . . . . .
C1 C 0.4832(4) 0.3517(4) 0.6401(3) 0.0323(10) Uani 1 1 d . . . . .
C2 C 0.4110(5) 0.2606(6) 0.6960(5) 0.067(2) Uani 1 1 d . . . . .
H2A H 0.366695 0.279301 0.729571 0.080 Uiso 1 1 calc R U . . .
H2B H 0.365160 0.199659 0.660913 0.080 Uiso 1 1 calc R U . . .
O2W O 0.220(4) 0.227(4) 0.500000 0.148(18) Uiso 0.3333 2 d S . P . .
O3W O 0.142(4) 0.155(4) 0.664(4) 0.174(17) Uiso 0.25 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tb1 0.0225(3) 0.0225(3) 0.0146(4) 0.000 0.000 0.01124(15)
Ni1 0.0249(6) 0.0248(6) 0.0160(6) 0.000 0.000 0.0164(5)
O1W 0.032(2) 0.040(3) 0.023(2) 0.000 0.000 0.024(2)
O3 0.027(3) 0.040(2) 0.025(2) 0.0135(16) 0.000 0.0136(14)
O1 0.0323(17) 0.043(2) 0.0250(17) 0.0103(16) 0.0007(15) 0.0203(16)
O2 0.035(2) 0.060(3) 0.053(2) 0.033(2) 0.0046(18) 0.026(2)
C1 0.033(3) 0.039(3) 0.028(2) 0.012(2) 0.003(2) 0.021(2)
C2 0.033(3) 0.083(5) 0.084(5) 0.062(4) 0.010(3) 0.029(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
Tb1 O3 2.471(6) 3_665 ?
Tb1 O3 2.472(6) . ?
Tb1 O3 2.471(6) 2_655 ?
Tb1 O1 2.400(4) 10_666 ?
Tb1 O1 2.400(4) 11_656 ?
Tb1 O1 2.400(4) 12_556 ?
Tb1 O1 2.400(4) 2_655 ?
Tb1 O1 2.400(4) 3_665 ?
Tb1 O1 2.400(4) . ?
Ni1 O1W 2.091(4) . ?
Ni1 O1W 2.091(4) 13_666 ?
Ni1 O2 2.025(3) . ?
Ni1 O2 2.025(4) 13_666 ?
Ni1 O2 2.025(3) 16_556 ?
Ni1 O2 2.025(3) 4_665 ?
O1W H1WA 0.8832 . ?
O1W H1WA 0.88(6) 16_556 ?
O1W H1WB 0.90(9) 16_556 ?
O1W H1WB 0.8973 . ?
O3 C2 1.385(6) . ?
O3 C2 1.385(6) 12_556 ?
O1 C1 1.256(6) . ?
O2 C1 1.250(6) . ?
C1 C2 1.495(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
O3 Tb1 O3 120.0 3_665 . ?
O3 Tb1 O3 120.0 2_655 . ?
O3 Tb1 O3 120.000(1) 2_655 3_665 ?
O1 Tb1 O3 136.37(10) 11_656 . ?
O1 Tb1 O3 63.31(9) 10_666 3_665 ?
O1 Tb1 O3 63.31(9) . . ?
O1 Tb1 O3 63.31(9) 12_556 . ?
O1 Tb1 O3 74.06(9) 3_665 2_655 ?
O1 Tb1 O3 63.31(9) 3_665 3_665 ?
O1 Tb1 O3 74.06(9) 2_655 . ?
O1 Tb1 O3 74.06(9) 10_666 . ?
O1 Tb1 O3 63.32(9) 11_656 2_655 ?
O1 Tb1 O3 74.06(9) 11_656 3_665 ?
O1 Tb1 O3 136.37(10) . 2_655 ?
O1 Tb1 O3 136.37(10) 2_655 3_665 ?
O1 Tb1 O3 136.37(10) 3_665 . ?
O1 Tb1 O3 136.37(10) 10_666 2_655 ?
O1 Tb1 O3 74.06(9) . 3_665 ?
O1 Tb1 O3 74.06(9) 12_556 2_655 ?
O1 Tb1 O3 63.32(9) 2_655 2_655 ?
O1 Tb1 O3 136.37(10) 12_556 3_665 ?
O1 Tb1 O1 87.3(2) . 10_666 ?
O1 Tb1 O1 78.52(15) 11_656 10_666 ?
O1 Tb1 O1 78.52(15) 12_556 10_666 ?
O1 Tb1 O1 87.3(2) 11_656 3_665 ?
O1 Tb1 O1 148.11(19) 2_655 10_666 ?
O1 Tb1 O1 78.52(15) 2_655 . ?
O1 Tb1 O1 126.63(17) 11_656 2_655 ?
O1 Tb1 O1 78.52(15) 11_656 12_556 ?
O1 Tb1 O1 87.3(2) 2_655 12_556 ?
O1 Tb1 O1 126.63(17) 12_556 . ?
O1 Tb1 O1 78.52(15) 2_655 3_665 ?
O1 Tb1 O1 148.12(19) 12_556 3_665 ?
O1 Tb1 O1 126.63(17) 3_665 10_666 ?
O1 Tb1 O1 78.52(15) 3_665 . ?
O1 Tb1 O1 148.11(19) 11_656 . ?
O1W Ni1 O1W 180.0 13_666 . ?
O2 Ni1 O1W 86.47(14) 4_665 . ?
O2 Ni1 O1W 86.47(14) . 13_666 ?
O2 Ni1 O1W 93.53(14) 16_556 . ?
O2 Ni1 O1W 93.53(14) 13_666 13_666 ?
O2 Ni1 O1W 86.47(14) 13_666 . ?
O2 Ni1 O1W 93.53(14) 4_665 13_666 ?
O2 Ni1 O1W 93.52(14) . . ?
O2 Ni1 O1W 86.47(14) 16_556 13_666 ?
O2 Ni1 O2 88.8(3) 4_665 13_666 ?
O2 Ni1 O2 91.2(3) 16_556 13_666 ?
O2 Ni1 O2 180.0(2) 16_556 4_665 ?
O2 Ni1 O2 91.2(3) 4_665 . ?
O2 Ni1 O2 180.0 13_666 . ?
O2 Ni1 O2 88.8(3) 16_556 . ?
Ni1 O1W H1WA 108.8(14) . 16_556 ?
Ni1 O1W H1WA 108.8 . . ?
Ni1 O1W H1WB 111.1 . . ?
Ni1 O1W H1WB 111(2) . 16_556 ?
H1WA O1W H1WA 124.4 . 16_556 ?
H1WA O1W H1WB 102.2 16_556 16_556 ?
H1WA O1W H1WB 24.9 . 16_556 ?
H1WA O1W H1WB 102.2 . . ?
H1WB O1W H1WA 24.9 . 16_556 ?
H1WB O1W H1WB 78.5 . 16_556 ?
C2 O3 Tb1 122.8(3) . . ?
C2 O3 Tb1 122.8(3) 12_556 . ?
C2 O3 C2 114.3(6) . 12_556 ?
C1 O1 Tb1 125.8(3) . . ?
C1 O2 Ni1 131.0(3) . . ?
O1 C1 C2 117.9(4) . . ?
O2 C1 O1 126.1(4) . . ?
O2 C1 C2 116.0(4) . . ?
O3 C2 C1 109.6(5) . . ?
O3 C2 H2A 109.7 . . ?
O3 C2 H2B 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?

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
Tb1 O3 C2 C1 0.8(8) . . . . ?
Tb1 O1 C1 O2 173.3(4) . . . . ?
Tb1 O1 C1 C2 -8.8(8) . . . . ?
Ni1 O2 C1 O1 1.2(9) . . . . ?
Ni1 O2 C1 C2 -176.7(5) . . . . ?
O1 C1 C2 O3 4.7(9) . . . . ?
O2 C1 C2 O3 -177.2(5) . . . . ?
C2 O3 C2 C1 -179.2(8) 12_556 . . . ?

_shelx_res_file                  
;
TITL TbNiODA in P6/mcc
    tbnioda.res
    created by SHELXL-2018/3 at 14:07:52 on 12-Mar-2020
REM P6/mcc (#192 in standard setting)
CELL 0.71073 14.553668 14.553668 15.631841 90 90 120
ZERR 2 0.000694 0.000694 0.000897 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Ni O Tb
UNIT 48 72 6 82 4

L.S. 50
PLAN  5
TEMP 25(2)
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\TbNiODA.hkl">
REM </olex2.extras>

WGHT    0.105700    5.855401
FVAR       1.88789
TB1   5    0.666667    0.333333    0.750000    10.16667    0.02248    0.02248 =
         0.01464    0.00000    0.00000    0.01124
NI1   3    0.500000    0.500000    0.500000    10.25000    0.02487    0.02479 =
         0.01602    0.00000    0.00000    0.01638
O1W   4    0.647704    0.508417    0.500000    10.50000    0.03219    0.03992 =
         0.02334    0.00000    0.00000    0.02410
AFIX   7
H1WA  2    0.657018    0.485926    0.450027    10.50000   -1.50000
H1WB  2    0.648241    0.460931    0.536304    10.50000   -1.50000
AFIX   0
O3    4    0.470575    0.235288    0.750000    10.50000    0.02726    0.04037 =
         0.02491    0.01351    0.00000    0.01363
O1    4    0.581144    0.385639    0.645184    11.00000    0.03225    0.04309 =
         0.02503    0.01028    0.00069    0.02027
O2    4    0.439108    0.385251    0.590628    11.00000    0.03458    0.06005 =
         0.05329    0.03282    0.00458    0.02567
C1    1    0.483230    0.351748    0.640147    11.00000    0.03271    0.03930 =
         0.02847    0.01192    0.00318    0.02066
C2    1    0.411007    0.260576    0.696025    11.00000    0.03339    0.08288 =
         0.08447    0.06165    0.00959    0.02878
AFIX  23
H2A   2    0.366695    0.279301    0.729571    11.00000   -1.20000
H2B   2    0.365160    0.199659    0.660913    11.00000   -1.20000
AFIX   0

O2W   4    0.219634    0.227147    0.500000    10.16667    0.14794
O3W   4    0.141887    0.155006    0.663990    10.25000    0.17360
HKLF 4




REM  TbNiODA in P6/mcc
REM wR2 = 0.1717, GooF = S = 1.138, Restrained GooF = 1.138 for all data
REM R1 = 0.0515 for 992 Fo > 4sig(Fo) and 0.0588 for all 1245 data
REM 62 parameters refined using 0 restraints

END

WGHT      0.1057      5.8557

REM Highest difference peak  2.704,  deepest hole -0.942,  1-sigma level  0.300
Q1    1   0.4241  0.4241  0.7500  10.50000  0.05    2.70
Q2    1   0.1296  0.1795  0.7498  11.00000  0.05    2.33
Q3    1   0.2687  0.1920  0.5000  10.50000  0.05    2.20
Q4    1   0.1889  0.2698  0.5000  10.50000  0.05    2.14
Q5    1   0.4892  0.2816  0.7500  11.00000  0.05    2.05
;
_shelx_res_checksum              79882
_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 1.096
_oxdiff_exptl_absorpt_empirical_full_min 0.897
####################################################################### 
# 
# 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_ybnioda
_database_code_depnum_ccdc_archive 'CCDC 1969723'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 Ni3 O36 Yb2, 3(O)'
_chemical_formula_sum            'C24 H36 Ni3 O39 Yb2'
_chemical_formula_weight         1470.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         Yb2Ni3C24H36O36
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'
Ni Ni 0.3393 1.1124 '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'
Yb Yb -0.3850 5.5486 '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      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   13.9032(4)
_cell_length_b                   13.9032(4)
_cell_length_c                   16.1471(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2703.05(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2726
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.0900
_cell_measurement_theta_min      2.5250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.549
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 5 0 0.0178
3 -5 0 0.0178
2 0 5 0.0350
-2 0 -5 0.0350
-5 -2 3 0.0187
5 2 -3 0.0187

_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.036
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
-2.9948 4.9962 0.0009 -0.0399 0.0808 0.2403
2.9948 -4.9962 -0.0009 0.0399 -0.0808 -0.2403
1.9983 0.0002 4.9926 0.1925 -0.1433 0.0658
-1.9983 -0.0002 -4.9926 -0.1925 0.1433 -0.0658
-4.9929 -1.9962 2.9965 -0.2700 -0.2812 -0.0152
4.9929 1.9962 -2.9965 0.2700 0.2812 0.0152

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6979
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.691
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -68.00   1.00   75.00    --  -29.32 178.00 -90.00   52
  2  ω    -96.00  23.00   1.00   75.00    --  -29.32   0.00-180.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0543398000
_diffrn_orient_matrix_UB_12      0.0245770000
_diffrn_orient_matrix_UB_13      0.0168118000
_diffrn_orient_matrix_UB_21      0.0220440000
_diffrn_orient_matrix_UB_22      0.0293968000
_diffrn_orient_matrix_UB_23      -0.0375336000
_diffrn_orient_matrix_UB_31      -0.0055972000
_diffrn_orient_matrix_UB_32      0.0447351000
_diffrn_orient_matrix_UB_33      0.0154132000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                909
_reflns_number_total             1168
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.502
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.094
_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)+(0.0636P)²+9.9855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1151
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.125) O3W(0.125)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.333333 0.666667 0.250000 0.01945(19) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.0188(3) Uani 1 4 d S T P . .
O3 O 0.5341(4) 0.7671(2) 0.250000 0.0305(11) Uani 1 2 d S T P . .
O1W O 0.3472(4) 0.4962(4) 0.500000 0.0278(10) Uani 1 2 d S T P . .
H1WA H 0.277330 0.421417 0.492009 0.042 Uiso 0.5 1 d R U P . .
H1WB H 0.335421 0.541878 0.456761 0.042 Uiso 0.5 1 d R U P . .
O1 O 0.4178(3) 0.6124(3) 0.3517(2) 0.0308(8) Uani 1 1 d . . . . .
O2 O 0.5660(3) 0.6210(3) 0.4129(2) 0.0383(9) Uani 1 1 d . . . . .
C1 C 0.5205(4) 0.6518(4) 0.3619(3) 0.0286(10) Uani 1 1 d . . . . .
C2 C 0.5973(5) 0.7488(7) 0.3093(5) 0.065(2) Uani 1 1 d . . . . .
H2A H 0.637914 0.814335 0.343601 0.078 Uiso 1 1 calc R U . . .
H2B H 0.650459 0.733649 0.281999 0.078 Uiso 1 1 calc R U . . .
O2W O 0.798(3) 0.795(3) 0.500000 0.083(11) Uiso 0.25 2 d S . P . .
O3W O 0.880(5) 0.862(5) 0.331(4) 0.096(17) Uiso 0.125 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Yb1 0.0223(2) 0.0223(2) 0.0138(3) 0.000 0.000 0.01113(11)
Ni1 0.0224(6) 0.0238(6) 0.0146(5) 0.000 0.000 0.0149(4)
O3 0.027(2) 0.036(2) 0.026(2) 0.0129(18) 0.000 0.0134(12)
O1W 0.024(2) 0.035(3) 0.028(2) 0.000 0.000 0.017(2)
O1 0.0291(17) 0.0374(19) 0.0264(16) 0.0095(15) -0.0005(14) 0.0170(17)
O2 0.0316(19) 0.049(2) 0.037(2) 0.0223(18) 0.0030(16) 0.0223(18)
C1 0.032(3) 0.033(3) 0.023(2) 0.009(2) 0.001(2) 0.018(2)
C2 0.040(3) 0.083(5) 0.066(5) 0.055(4) 0.002(3) 0.026(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
Yb1 O3 2.418(5) 3_565 ?
Yb1 O3 2.418(5) . ?
Yb1 O3 2.418(5) 2_665 ?
Yb1 O1 2.352(3) 3_565 ?
Yb1 O1 2.352(3) 12_565 ?
Yb1 O1 2.352(3) 11 ?
Yb1 O1 2.352(3) . ?
Yb1 O1 2.352(3) 10_665 ?
Yb1 O1 2.352(3) 2_665 ?
Ni1 O1W 2.098(4) . ?
Ni1 O1W 2.098(4) 13_666 ?
Ni1 O2 2.027(4) 16_556 ?
Ni1 O2 2.027(4) . ?
Ni1 O2 2.027(4) 13_666 ?
Ni1 O2 2.027(4) 4_665 ?
O3 C2 1.406(6) . ?
O3 C2 1.406(6) 12_565 ?
O1W H1WA 1.0156 . ?
O1W H1WB 1.0108 . ?
O1 C1 1.258(6) . ?
O2 C1 1.238(6) . ?
C1 C2 1.496(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O3W O3W 1.81(6) 5_565 ?
O3W O3W 1.81(6) 6_655 ?

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
O3 Yb1 O3 120.0 3_565 . ?
O3 Yb1 O3 119.999(1) 2_665 . ?
O3 Yb1 O3 120.0 2_665 3_565 ?
O1 Yb1 O3 73.86(9) 11 3_565 ?
O1 Yb1 O3 73.86(9) 10_665 . ?
O1 Yb1 O3 135.26(10) 10_665 2_665 ?
O1 Yb1 O3 135.26(10) 2_665 3_565 ?
O1 Yb1 O3 135.26(10) 11 . ?
O1 Yb1 O3 64.38(8) 2_665 2_665 ?
O1 Yb1 O3 64.39(8) 10_665 3_565 ?
O1 Yb1 O3 64.39(8) 11 2_665 ?
O1 Yb1 O3 64.39(8) . . ?
O1 Yb1 O3 135.26(10) . 2_665 ?
O1 Yb1 O3 64.39(8) 12_565 . ?
O1 Yb1 O3 135.26(10) 3_565 . ?
O1 Yb1 O3 73.86(9) 3_565 2_665 ?
O1 Yb1 O3 73.86(9) 12_565 2_665 ?
O1 Yb1 O3 64.38(8) 3_565 3_565 ?
O1 Yb1 O3 135.26(10) 12_565 3_565 ?
O1 Yb1 O3 73.86(9) 2_665 . ?
O1 Yb1 O3 73.86(9) . 3_565 ?
O1 Yb1 O1 147.72(17) 11 . ?
O1 Yb1 O1 76.63(15) 11 10_665 ?
O1 Yb1 O1 128.77(16) 3_565 10_665 ?
O1 Yb1 O1 128.77(16) 11 2_665 ?
O1 Yb1 O1 147.72(17) 2_665 10_665 ?
O1 Yb1 O1 76.63(15) 2_665 3_565 ?
O1 Yb1 O1 76.63(15) 2_665 . ?
O1 Yb1 O1 89.48(19) . 10_665 ?
O1 Yb1 O1 76.63(15) 11 12_565 ?
O1 Yb1 O1 89.48(19) 2_665 12_565 ?
O1 Yb1 O1 128.77(16) 12_565 . ?
O1 Yb1 O1 89.48(19) 11 3_565 ?
O1 Yb1 O1 76.63(15) 12_565 10_665 ?
O1 Yb1 O1 76.63(15) 3_565 . ?
O1 Yb1 O1 147.72(17) 12_565 3_565 ?
O1W Ni1 O1W 180.0 13_666 . ?
O2 Ni1 O1W 93.04(14) 16_556 . ?
O2 Ni1 O1W 86.96(14) 16_556 13_666 ?
O2 Ni1 O1W 86.96(14) 13_666 . ?
O2 Ni1 O1W 93.04(14) . . ?
O2 Ni1 O1W 93.04(14) 4_665 13_666 ?
O2 Ni1 O1W 93.04(14) 13_666 13_666 ?
O2 Ni1 O1W 86.96(14) . 13_666 ?
O2 Ni1 O1W 86.96(14) 4_665 . ?
O2 Ni1 O2 92.1(2) . 4_665 ?
O2 Ni1 O2 180.0(2) 16_556 4_665 ?
O2 Ni1 O2 87.9(2) 4_665 13_666 ?
O2 Ni1 O2 180.0 . 13_666 ?
O2 Ni1 O2 87.9(2) . 16_556 ?
O2 Ni1 O2 92.1(2) 16_556 13_666 ?
C2 O3 Yb1 122.7(3) . . ?
C2 O3 Yb1 122.7(3) 12_565 . ?
C2 O3 C2 114.5(6) . 12_565 ?
Ni1 O1W H1WA 117.6 . . ?
Ni1 O1W H1WB 117.7 . . ?
H1WA O1W H1WB 100.5 . . ?
C1 O1 Yb1 126.2(3) . . ?
C1 O2 Ni1 130.6(3) . . ?
O1 C1 C2 117.6(4) . . ?
O2 C1 O1 126.9(5) . . ?
O2 C1 C2 115.5(5) . . ?
O3 C2 C1 108.7(5) . . ?
O3 C2 H2A 110.0 . . ?
O3 C2 H2B 110.0 . . ?
C1 C2 H2A 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
O3W O3W O3W 120.00(5) 5_565 6_655 ?

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
Yb1 O3 C2 C1 6.6(8) . . . . ?
Yb1 O1 C1 O2 -176.8(4) . . . . ?
Yb1 O1 C1 C2 5.4(8) . . . . ?
Ni1 O2 C1 O1 -0.7(9) . . . . ?
Ni1 O2 C1 C2 177.2(5) . . . . ?
O1 C1 C2 O3 -7.3(9) . . . . ?
O2 C1 C2 O3 174.6(5) . . . . ?
C2 O3 C2 C1 -173.4(8) 12_565 . . . ?

_shelx_res_file                  
;
TITL ybnioda_c.res in P6/mcc
    ybnioda.res
    created by SHELXL-2018/3 at 12:44:14 on 12-Mar-2020
REM Old TITL ybnioda_c.res in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.303, Rweak 0.004, Alpha 0.069, Orientation as input
REM Formula found by SHELXT: C88 O6 Ni8 Yb
CELL 0.71073 13.9032 13.9032 16.1471 90 90 120
ZERR 2 0.0004 0.0004 0.0004 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H Ni O Yb
UNIT 48 72 6 78 4

L.S. 30
PLAN  3
TEMP 25(2)
CONF
BOND $H
LIST 6
MORE -1
fmap 2
acta
OMIT 5 0 2
OMIT 2 1 0
OMIT 0 0 2
OMIT 2 2 0
OMIT 4 1 2
OMIT 0 0 4
OMIT 1 0 0
OMIT 4 0 2
OMIT 3 0 0
REM <olex2.extras>
REM <HklSrc "%.\\YbNiODA.hkl">
REM </olex2.extras>

WGHT    0.063600    9.985499
FVAR       0.23081
YB1   5    0.333333    0.666667    0.250000    10.16667    0.02227    0.02227 =
         0.01382    0.00000    0.00000    0.01113
NI1   3    0.500000    0.500000    0.500000    10.25000    0.02240    0.02376 =
         0.01464    0.00000    0.00000    0.01487
O3    4    0.534148    0.767074    0.250000    10.50000    0.02679    0.03590 =
         0.02586    0.01290    0.00000    0.01340
O1W   4    0.347210    0.496197    0.500000    10.50000    0.02398    0.03477 =
         0.02798    0.00000    0.00000    0.01724
AFIX   7
H1WA  2    0.277330    0.421417    0.492009    10.50000   -1.50000
H1WB  2    0.335421    0.541878    0.456761    10.50000   -1.50000
AFIX   0
O1    4    0.417792    0.612354    0.351717    11.00000    0.02909    0.03741 =
         0.02643    0.00952   -0.00048    0.01701
O2    4    0.565975    0.621041    0.412863    11.00000    0.03156    0.04919 =
         0.03690    0.02231    0.00301    0.02228
C1    1    0.520457    0.651843    0.361879    11.00000    0.03242    0.03297 =
         0.02294    0.00868    0.00125    0.01821
C2    1    0.597300    0.748773    0.309350    11.00000    0.03956    0.08344 =
         0.06591    0.05487    0.00195    0.02622
AFIX  23
H2A   2    0.637914    0.814335    0.343601    11.00000   -1.20000
H2B   2    0.650459    0.733649    0.281999    11.00000   -1.20000
AFIX   0

O2W   4    0.797736    0.795189    0.500000    10.12500    0.08333
O3W   4    0.879893    0.861521    0.330987    10.12500    0.09600
HKLF 4




REM  ybnioda_c.res in P6/mcc
REM wR2 = 0.1151, GooF = S = 1.094, Restrained GooF = 1.094 for all data
REM R1 = 0.0322 for 909 Fo > 4sig(Fo) and 0.0428 for all 1168 data
REM 62 parameters refined using 0 restraints

END

WGHT      0.0636      9.9856

REM Highest difference peak  1.502,  deepest hole -0.782,  1-sigma level  0.176
Q1    1   0.7988  0.7927  0.5405  11.00000  0.05    1.50
Q2    1   0.8612  0.8789  0.2925  11.00000  0.05    0.74
Q3    1   0.9205  0.8399  0.2867  11.00000  0.05    0.62
;
_shelx_res_checksum              84164
_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 1.080
_oxdiff_exptl_absorpt_empirical_full_min 0.939
####################################################################### 
# 
# 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_lanioda
_database_code_depnum_ccdc_archive 'CCDC 1969724'
loop_
_audit_author_name
_audit_author_address
'Javier Gonzalez-Platas'
;Universidad de La Laguna
Spain
;
_audit_update_record             
;
2020-03-12 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H36 La2 Ni3 O36, 3(O)'
_chemical_formula_sum            'C24 H36 La2 Ni3 O39'
_chemical_formula_weight         1402.48
_chemical_melting_point          ?
_chemical_oxdiff_formula         La2Ni3C24H36O36
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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   15.3094(3)
_cell_length_b                   15.3094(3)
_cell_length_c                   15.0182(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3048.35(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4360
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.8330
_cell_measurement_theta_min      2.6510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.367
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1380
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0356
-1 1 0 0.0150
-4 -4 5 0.0487
4 4 -5 0.0487
-1 -1 0 0.0296
1 1 0 0.0296
2 -2 5 0.0686
5 0 2 0.0335
5 1 1 0.0252
5 -2 0 0.0302
-5 2 0 0.0184
5 -2 -3 0.0451

_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.049
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
1.0000 -0.9986 0.0011 0.0022 -0.0534 -0.0002
-1.0000 0.9986 -0.0011 -0.0022 0.0534 0.0002
-3.9945 -3.9978 4.9977 0.0184 0.0024 -0.4388
3.9945 3.9978 -4.9977 -0.0184 -0.0024 0.4388
-0.9967 -1.0013 -0.0001 0.0530 0.0024 -0.0759
0.9967 1.0013 0.0001 -0.0530 -0.0024 0.0759
1.9922 -1.9897 5.0002 -0.1890 -0.1141 -0.1356
4.9885 0.0098 2.0021 -0.2043 -0.1425 0.1352
4.9884 1.0083 1.0020 -0.1932 -0.1155 0.2003
4.9949 -1.9930 0.0039 -0.0718 -0.1906 0.1132
-4.9949 1.9930 -0.0039 0.0718 0.1906 -0.1132
4.9995 -1.9974 -2.9950 0.0442 -0.1862 0.1943

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.661
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     69.00 117.00   1.00   30.00    --   28.54 178.00   0.00   48
  2  ω    -71.00  25.00   1.00   30.00    --  -29.17 -19.00 -60.00   96
  3  ω   -105.00  10.00   1.00   30.00    --  -29.17   0.00-150.00  115
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0253682000
_diffrn_orient_matrix_UB_12      -0.0276303000
_diffrn_orient_matrix_UB_13      -0.0386885000
_diffrn_orient_matrix_UB_21      -0.0279946000
_diffrn_orient_matrix_UB_22      0.0254541000
_diffrn_orient_matrix_UB_23      -0.0015373000
_diffrn_orient_matrix_UB_31      0.0378816000
_diffrn_orient_matrix_UB_32      0.0380869000
_diffrn_orient_matrix_UB_33      -0.0270467000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1097
_reflns_number_total             1322
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.104
_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)+(0.0668P)²+8.8824P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1247
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O(0.16667) O4(0.08333)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.666667 0.333333 0.750000 0.01664(19) Uani 1 6 d S T P . .
Ni1 Ni 0.500000 0.000000 0.500000 0.0182(2) Uani 1 4 d S T P . .
O1W O 0.6406(3) 0.1317(3) 0.500000 0.0240(8) Uani 1 2 d S T P . .
H1WA H 0.684777 0.120637 0.524684 0.036 Uiso 0.5 1 d R U P . .
H1WB H 0.638962 0.176213 0.533553 0.036 Uiso 0.5 1 d R U P . .
O1 O 0.5746(2) 0.1926(2) 0.6415(2) 0.0319(7) Uani 1 1 d . . . . .
O2 O 0.4408(2) 0.0505(2) 0.5952(2) 0.0432(9) Uani 1 1 d . . . . .
O3 O 0.4712(3) 0.23561(15) 0.750000 0.0314(10) Uani 1 2 d S T P . .
C1 C 0.4823(3) 0.1289(3) 0.6407(3) 0.0299(9) Uani 1 1 d . . . . .
C2 C 0.4142(4) 0.1477(4) 0.7001(4) 0.0607(19) Uani 1 1 d . . . . .
H2A H 0.365418 0.154674 0.664129 0.073 Uiso 1 1 calc R U . . .
H2B H 0.377694 0.090779 0.739824 0.073 Uiso 1 1 calc R U . . .
O O 0.784(3) 0.042(3) 0.500000 0.141(11) Uiso 0.3333 2 d S . P . .
O4 O 1.018(3) 0.170(4) 0.684(3) 0.054(11) Uiso 0.0833 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
La1 0.0177(2) 0.0177(2) 0.0145(3) 0.000 0.000 0.00885(11)
Ni1 0.0221(5) 0.0145(4) 0.0166(4) 0.000 0.000 0.0080(4)
O1W 0.025(2) 0.0202(18) 0.0247(18) 0.000 0.000 0.0102(16)
O1 0.0259(14) 0.0314(15) 0.0310(14) -0.0159(13) 0.0008(12) 0.0088(12)
O2 0.0282(16) 0.0356(18) 0.052(2) -0.0265(16) 0.0068(15) 0.0057(14)
O3 0.0221(19) 0.0301(16) 0.039(2) -0.0207(16) 0.000 0.0110(10)
C1 0.026(2) 0.028(2) 0.032(2) -0.0130(18) 0.0004(17) 0.0106(17)
C2 0.025(2) 0.054(3) 0.082(4) -0.053(3) 0.006(3) 0.004(2)

_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
La1 O1 2.500(3) 2_655 ?
La1 O1 2.500(3) 10_666 ?
La1 O1 2.500(3) 11_656 ?
La1 O1 2.500(3) 12_556 ?
La1 O1 2.500(3) 3_665 ?
La1 O1 2.499(3) . ?
La1 O3 2.591(4) 3_665 ?
La1 O3 2.591(4) 2_655 ?
La1 O3 2.591(4) . ?
Ni1 O1W 2.088(4) . ?
Ni1 O1W 2.088(4) 13_656 ?
Ni1 O2 2.040(3) . ?
Ni1 O2 2.040(3) 13_656 ?
Ni1 O2 2.040(3) 16_556 ?
Ni1 O2 2.040(3) 4_655 ?
O1W H1WA 0.8585 . ?
O1W H1WA 0.86(5) 16_556 ?
O1W H1WB 0.86(6) 16_556 ?
O1W H1WB 0.8582 . ?
O1 C1 1.253(5) . ?
O2 C1 1.245(5) . ?
O3 C2 1.400(5) 12_556 ?
O3 C2 1.400(5) . ?
C1 C2 1.505(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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 La1 O1 82.10(11) 2_655 . ?
O1 La1 O1 121.56(13) 10_666 3_665 ?
O1 La1 O1 82.10(11) 10_666 12_556 ?
O1 La1 O1 150.04(14) 11_656 3_665 ?
O1 La1 O1 121.57(13) . 12_556 ?
O1 La1 O1 82.10(11) 11_656 12_556 ?
O1 La1 O1 83.40(15) 2_655 10_666 ?
O1 La1 O1 121.56(13) 2_655 11_656 ?
O1 La1 O1 150.04(14) . 10_666 ?
O1 La1 O1 150.04(14) 2_655 12_556 ?
O1 La1 O1 82.10(11) 11_656 10_666 ?
O1 La1 O1 83.40(15) . 11_656 ?
O1 La1 O1 82.10(11) 2_655 3_665 ?
O1 La1 O1 82.10(11) . 3_665 ?
O1 La1 O1 83.40(15) 3_665 12_556 ?
O1 La1 O3 60.78(6) 2_655 2_655 ?
O1 La1 O3 138.30(8) 3_665 2_655 ?
O1 La1 O3 138.30(8) 2_655 . ?
O1 La1 O3 75.02(7) 11_656 . ?
O1 La1 O3 138.30(8) 12_556 2_655 ?
O1 La1 O3 138.30(8) . 3_665 ?
O1 La1 O3 75.02(7) 12_556 3_665 ?
O1 La1 O3 75.02(7) . 2_655 ?
O1 La1 O3 75.02(7) 2_655 3_665 ?
O1 La1 O3 60.78(7) 12_556 . ?
O1 La1 O3 138.30(8) 11_656 3_665 ?
O1 La1 O3 60.78(6) 11_656 2_655 ?
O1 La1 O3 60.78(7) . . ?
O1 La1 O3 75.02(7) 10_666 2_655 ?
O1 La1 O3 75.02(7) 3_665 . ?
O1 La1 O3 138.30(8) 10_666 . ?
O1 La1 O3 60.78(7) 3_665 3_665 ?
O1 La1 O3 60.78(6) 10_666 3_665 ?
O3 La1 O3 120.0 2_655 . ?
O3 La1 O3 120.000(1) 2_655 3_665 ?
O3 La1 O3 120.0 . 3_665 ?
O1W Ni1 O1W 180.0 13_656 . ?
O2 Ni1 O1W 94.20(11) 4_655 13_656 ?
O2 Ni1 O1W 94.20(11) . . ?
O2 Ni1 O1W 85.80(11) 13_656 . ?
O2 Ni1 O1W 85.80(11) 16_556 13_656 ?
O2 Ni1 O1W 94.20(11) 13_656 13_656 ?
O2 Ni1 O1W 85.80(11) . 13_656 ?
O2 Ni1 O1W 94.20(11) 16_556 . ?
O2 Ni1 O1W 85.80(11) 4_655 . ?
O2 Ni1 O2 180.0 13_656 . ?
O2 Ni1 O2 91.0(2) 16_556 13_656 ?
O2 Ni1 O2 89.0(2) 4_655 13_656 ?
O2 Ni1 O2 91.0(2) 4_655 . ?
O2 Ni1 O2 89.0(2) 16_556 . ?
O2 Ni1 O2 180.00(14) 16_556 4_655 ?
Ni1 O1W H1WA 110.0(12) . 16_556 ?
Ni1 O1W H1WA 110.0 . . ?
Ni1 O1W H1WB 109.9 . . ?
Ni1 O1W H1WB 109.9(14) . 16_556 ?
H1WA O1W H1WA 51.2 . 16_556 ?
H1WA O1W H1WB 104.0 16_556 16_556 ?
H1WA O1W H1WB 138.5 . 16_556 ?
H1WA O1W H1WB 104.0 . . ?
H1WB O1W H1WA 138.5 . 16_556 ?
H1WB O1W H1WB 71.9 . 16_556 ?
C1 O1 La1 127.4(3) . . ?
C1 O2 Ni1 129.9(3) . . ?
C2 O3 La1 122.7(2) 12_556 . ?
C2 O3 La1 122.7(2) . . ?
C2 O3 C2 114.7(5) 12_556 . ?
O1 C1 C2 117.7(4) . . ?
O2 C1 O1 126.1(4) . . ?
O2 C1 C2 116.2(4) . . ?
O3 C2 C1 110.0(4) . . ?
O3 C2 H2A 109.7 . . ?
O3 C2 H2B 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?

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
La1 O1 C1 O2 -167.8(4) . . . . ?
La1 O1 C1 C2 12.0(7) . . . . ?
La1 O3 C2 C1 -7.1(6) . . . . ?
Ni1 O2 C1 O1 -5.3(8) . . . . ?
Ni1 O2 C1 C2 174.9(4) . . . . ?
O1 C1 C2 O3 -2.4(7) . . . . ?
O2 C1 C2 O3 177.3(4) . . . . ?
C2 O3 C2 C1 172.9(6) 12_556 . . . ?

_shelx_res_file                  
;
TITL lanioda_a.res in P6/mcc
    lanioda.res
    created by SHELXL-2018/3 at 11:31:28 on 12-Mar-2020
REM Old TITL LaNiODA in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.079, Rweak 0.008, Alpha 0.047, Orientation as input
REM Formula found by SHELXT: C24 O36 Ni3 La2
CELL 0.71073 15.3094 15.3094 15.0182 90 90 120
ZERR 2 0.0003 0.0003 0.0003 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X+Y,+Z
SYMM -Y+X,+X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM -Y,-X,0.5-Z
SYMM +Y-X,+Y,0.5-Z
SYMM +X,+X-Y,0.5-Z
SFAC C H La Ni O
UNIT 48 72 4 6 78

L.S. 50
PLAN  6
TEMP 25(2)
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
OMIT 0 0 2
OMIT 2 1 0
OMIT 3 1 2
OMIT 1 1 0
OMIT 4 0 4
OMIT 4 0 2
OMIT 2 2 0
REM <olex2.extras>
REM <HklSrc "%.\\LaNiODA.hkl">
REM </olex2.extras>

WGHT    0.066800    8.882400
FVAR       0.23090
LA1   3    0.666667    0.333333    0.750000    10.16667    0.01769    0.01769 =
         0.01453    0.00000    0.00000    0.00885
NI1   4    0.500000    0.000000    0.500000    10.25000    0.02213    0.01447 =
         0.01655    0.00000    0.00000    0.00797
O1W   5    0.640642    0.131700    0.500000    10.50000    0.02545    0.02016 =
         0.02475    0.00000    0.00000    0.01022
AFIX   7
H1WA  2    0.684777    0.120637    0.524684    10.50000   -1.50000
H1WB  2    0.638962    0.176213    0.533553    10.50000   -1.50000
AFIX   0
O1    5    0.574646    0.192578    0.641504    11.00000    0.02592    0.03140 =
         0.03100   -0.01594    0.00075    0.00884
O2    5    0.440808    0.050457    0.595205    11.00000    0.02820    0.03560 =
         0.05210   -0.02645    0.00682    0.00570
O3    5    0.471218    0.235609    0.750000    10.50000    0.02210    0.03012 =
         0.03925   -0.02071    0.00000    0.01105
C1    1    0.482311    0.128926    0.640696    11.00000    0.02619    0.02780 =
         0.03171   -0.01299    0.00044    0.01056
C2    1    0.414216    0.147695    0.700083    11.00000    0.02522    0.05351 =
         0.08245   -0.05300    0.00603    0.00409
AFIX  23
H2A   2    0.365418    0.154674    0.664129    11.00000   -1.20000
H2B   2    0.377694    0.090779    0.739824    11.00000   -1.20000
AFIX   0

O     5    0.783633    0.042433    0.500000    10.16667    0.14083
O4    5    1.018411    0.170310    0.684014    10.08333    0.05374
HKLF 4




REM  lanioda_a.res in P6/mcc
REM wR2 = 0.1247, GooF = S = 1.104, Restrained GooF = 1.104 for all data
REM R1 = 0.0355 for 1097 Fo > 4sig(Fo) and 0.0443 for all 1322 data
REM 62 parameters refined using 0 restraints

END

WGHT      0.0663      8.9688

REM Highest difference peak  1.133,  deepest hole -0.730,  1-sigma level  0.130
Q1    1   0.7534 -0.0236  0.5000  10.50000  0.05    1.13
Q2    1   1.0000  0.0000  0.5000  10.08333  0.05    0.78
Q3    1   0.8139  0.1048  0.5000  10.50000  0.05    0.66
Q4    1   0.7990  0.0803  0.5407  11.00000  0.05    0.65
Q5    1   1.0841  0.1791  0.6310  11.00000  0.05    0.47
Q6    1   0.9822  0.1429  0.7383  11.00000  0.05    0.45
;
_shelx_res_checksum              33796
_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 1.257
_oxdiff_exptl_absorpt_empirical_full_min 0.890
####################################################################### 
# 
# 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_cu_191127_LS_JT_EuNioda_0m_b
_database_code_depnum_ccdc_archive 'CCDC 1987753'
loop_
_audit_author_name
_audit_author_address
'Leopoldo Suescun'
;Facultad de Quimica, Universidad de la Republica, Uruguay
Uruguay
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: The only crystal found suitable for diffraction to the required
resolution was split into two domains separated by less than 1 degree. It 
was impossible to integrate the data using a twin strategy therefore data
integration was performed as if the crystal was single-domain leading to
an important number of intensities that are not consistent, increasing 
the Rint value.
;
_vrf_PLAT417_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Short Inter D-H..H-D       H1       ..H1       .       1.34 Ang.  
RESPONSE: This is not an intermolecular H-H distance but intramolecular in
a water molecule placed over a mirror plane.
;
_vrf_PLAT601_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        439 Ang**3
RESPONSE: This compound is a MOF with large voids occupied by disordered 
solvent molecules that were partially modelled.
;
_vrf_PLAT094_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.40 Report
RESPONSE: There is a large value of positive residual density inside the 
compound's voids corresponding to disordered water molecules that cannot be 
suitably modelled.
;
_vrf_PLAT202_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check 
RESPONSE: These corresponds to the solvent molecules (O2W) filling 
the MOF's voids, which could only be modelled isotropically due to its 
high disorder.
;
_vrf_PLAT241_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: High   MainMol Ueq as Compared to Neighbors of         O2 Check   
RESPONSE: The oxidiacetate ligand possesses a slight disorder that 
enhances the Ueq of the light elements in comparison to that of Ni atoms, 
which lie in special positions. Such disorder is not enough to justify a 
splitting in the case of O2, but it is enough to generate an appreciable 
difference of U against Ni.
;
_vrf_PLAT242_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Low    MainMol Ueq as Compared to Neighbors of        Eu1 Check   
RESPONSE: The oxidiacetate ligand possesses a slight disorder that 
enhances the Ueq of the light elements in comparison to that of Eu atoms, 
which lie in special positions. Such disorder is not enough to justify a 
splitting in the case of O2, but it is enough to generate an appreciable 
difference of U against Ni.
;
_vrf_PLAT906_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Large K Value in the Analysis of Variance ......     17.066 Check 
RESPONSE: It is a frequent problem of area detectors to overestimate the
background and let some low intensity reflections underestimated. For this
reason, for a small number of low intensity reflections below 1% of Fcmax
a rather large K value is found.
;
_vrf_PLAT973_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Check Calcd Positive Resid. Density on       Eu1       1.14 eA-3  
RESPONSE: Poor data quality, due to split crystal and poor scattering power 
of the very small domains made the calculated electron density deviate from
the expected values.
;
_vrf_PLAT975_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Check Calcd Resid. Dens.  0.76A   From O2W             0.63 eA-3  
RESPONSE: O2W corresponds to a fairly disorder water molecule inside the
compound's voids, this causes the appearance of residual electron density 
surrounding the atom.
;
_vrf_PLAT976_cu_191127_LS_JT_EuNioda_0m_b 
;
PROBLEM: Check Calcd Resid. Dens.  0.93A   From O2W            -0.42 eA-3  
RESPONSE: O2W corresponds to a fairly disorder water molecule inside the
compound's voids, this causes the appearance of residual electron density 
surrounding the atom.
;
# end Validation Reply Form


_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            'C24 H36 Eu2 Ni3 O40.56'
_chemical_formula_weight         1453.54

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'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   14.5288(9)
_cell_length_b                   14.5288(9)
_cell_length_c                   15.6072(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2853.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1036
_cell_measurement_theta_min      3.98
_cell_measurement_theta_max      22.05

_exptl_crystal_description       'hexagonal needle'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_F_000             1429
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.056
_exptl_absorpt_coefficient_mu    17.440
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  0.3295
_exptl_absorpt_correction_T_min  0.1405
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 10.83333
_diffrn_reflns_number            28180
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_av_R_equivalents  0.1478
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.513
_diffrn_reflns_theta_max         76.272
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1043
_reflns_number_gt                823
_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.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'split crystal'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0882P)²+3.7563P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00082(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1043
_refine_ls_number_parameters     72
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1576
_refine_ls_wR_factor_gt          0.1442
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.130
_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
Eu1 Eu 0.666667 0.333333 0.250000 0.0333(4) Uani 1 6 d S T P A .
Ni1 Ni 0.500000 0.500000 0.500000 0.0371(5) Uani 1 4 d S T P . .
O1 O 0.5797(4) 0.3858(4) 0.3552(3) 0.0503(11) Uani 1 1 d . . . . .
C1 C 0.4806(5) 0.3512(5) 0.3608(4) 0.0516(15) Uani 1 1 d . . . . .
O2 O 0.4378(4) 0.3847(4) 0.4093(3) 0.0630(13) Uani 1 1 d . . . . .
C2A C 0.415(3) 0.285(3) 0.284(3) 0.054(6) Uani 0.35(4) 1 d . U P A 1
H2AA H 0.343706 0.232093 0.302312 0.064 Uiso 0.35(4) 1 calc R U P A 1
H2AB H 0.409085 0.329820 0.241126 0.064 Uiso 0.35(4) 1 calc R U P A 1
C2B C 0.4065(14) 0.2496(17) 0.3126(15) 0.053(4) Uani 0.65(4) 1 d . U P A 2
H2BA H 0.374796 0.189824 0.351726 0.064 Uiso 0.65(4) 1 calc R U P A 2
H2BB H 0.350002 0.256103 0.285282 0.064 Uiso 0.65(4) 1 calc R U P A 2
O1W O 0.3527(5) 0.4932(5) 0.500000 0.0451(14) Uani 1 2 d S T P . .
O3 O 0.4682(5) 0.2341(3) 0.250000 0.0489(16) Uani 1 2 d S T P . .
H1 H 0.353(8) 0.537(8) 0.457(6) 0.10(3) Uiso 1 1 d . . . . .
O2W O 0.207(5) 0.236(4) 0.500000 0.35(3) Uiso 0.76 2 d S . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Eu1 0.0360(4) 0.0360(4) 0.0278(5) 0.000 0.000 0.0180(2)
Ni1 0.0394(11) 0.0436(11) 0.0344(10) 0.000 0.000 0.0254(9)
O1 0.050(2) 0.060(3) 0.045(2) -0.012(2) 0.0002(19) 0.030(2)
C1 0.051(4) 0.056(4) 0.053(4) -0.011(3) -0.002(3) 0.031(3)
O2 0.050(3) 0.076(3) 0.068(3) -0.024(3) -0.002(2) 0.035(3)
C2A 0.047(8) 0.052(13) 0.062(14) -0.014(9) 0.008(10) 0.024(10)
C2B 0.044(5) 0.050(10) 0.061(11) -0.009(7) 0.004(7) 0.021(7)
O1W 0.049(3) 0.054(4) 0.041(3) 0.000 0.000 0.032(3)
O3 0.041(3) 0.054(3) 0.048(3) -0.016(2) 0.000 0.0204(17)

_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
Eu1 O1 2.416(4) 12 ?
Eu1 O1 2.416(4) 3_665 ?
Eu1 O1 2.416(4) 11_655 ?
Eu1 O1 2.416(4) 2_655 ?
Eu1 O1 2.416(4) 10_665 ?
Eu1 O1 2.416(4) . ?
Eu1 O3 2.498(7) 2_655 ?
Eu1 O3 2.498(7) 3_665 ?
Eu1 O3 2.498(7) . ?
Ni1 O2 2.028(5) 13_666 ?
Ni1 O2 2.028(5) 16_556 ?
Ni1 O2 2.028(5) 4_665 ?
Ni1 O2 2.028(5) . ?
Ni1 O1W 2.092(6) 13_666 ?
Ni1 O1W 2.092(6) . ?
O1 C1 1.269(8) . ?
C1 O2 1.224(8) . ?
C1 C2B 1.522(18) . ?
C1 C2A 1.54(4) . ?
C2A O3 1.41(3) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2B O3 1.418(18) . ?
C2B H2BA 0.9700 . ?
C2B H2BB 0.9700 . ?
O1W H1 0.92(10) . ?

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 Eu1 O1 148.3(2) 12 3_665 ?
O1 Eu1 O1 78.86(18) 12 11_655 ?
O1 Eu1 O1 86.9(2) 3_665 11_655 ?
O1 Eu1 O1 86.9(2) 12 2_655 ?
O1 Eu1 O1 78.86(18) 3_665 2_655 ?
O1 Eu1 O1 126.1(2) 11_655 2_655 ?
O1 Eu1 O1 78.86(18) 12 10_665 ?
O1 Eu1 O1 126.1(2) 3_665 10_665 ?
O1 Eu1 O1 78.86(18) 11_655 10_665 ?
O1 Eu1 O1 148.3(2) 2_655 10_665 ?
O1 Eu1 O1 126.1(2) 12 . ?
O1 Eu1 O1 78.86(18) 3_665 . ?
O1 Eu1 O1 148.3(2) 11_655 . ?
O1 Eu1 O1 78.85(18) 2_655 . ?
O1 Eu1 O1 86.9(2) 10_665 . ?
O1 Eu1 O3 74.15(11) 12 2_655 ?
O1 Eu1 O3 74.15(11) 3_665 2_655 ?
O1 Eu1 O3 63.07(10) 11_655 2_655 ?
O1 Eu1 O3 63.07(10) 2_655 2_655 ?
O1 Eu1 O3 136.55(12) 10_665 2_655 ?
O1 Eu1 O3 136.55(12) . 2_655 ?
O1 Eu1 O3 136.55(12) 12 3_665 ?
O1 Eu1 O3 63.07(10) 3_665 3_665 ?
O1 Eu1 O3 74.15(11) 11_655 3_665 ?
O1 Eu1 O3 136.55(12) 2_655 3_665 ?
O1 Eu1 O3 63.07(11) 10_665 3_665 ?
O1 Eu1 O3 74.15(11) . 3_665 ?
O3 Eu1 O3 120.000(1) 2_655 3_665 ?
O1 Eu1 O3 63.07(11) 12 . ?
O1 Eu1 O3 136.55(12) 3_665 . ?
O1 Eu1 O3 136.55(12) 11_655 . ?
O1 Eu1 O3 74.15(11) 2_655 . ?
O1 Eu1 O3 74.15(11) 10_665 . ?
O1 Eu1 O3 63.07(11) . . ?
O3 Eu1 O3 120.0 2_655 . ?
O3 Eu1 O3 120.000(1) 3_665 . ?
O2 Ni1 O2 91.4(3) 13_666 16_556 ?
O2 Ni1 O2 88.6(3) 13_666 4_665 ?
O2 Ni1 O2 180.0(3) 16_556 4_665 ?
O2 Ni1 O2 180.0 13_666 . ?
O2 Ni1 O2 88.6(3) 16_556 . ?
O2 Ni1 O2 91.4(3) 4_665 . ?
O2 Ni1 O1W 86.44(18) 13_666 13_666 ?
O2 Ni1 O1W 93.56(18) 16_556 13_666 ?
O2 Ni1 O1W 86.44(18) 4_665 13_666 ?
O2 Ni1 O1W 93.56(18) . 13_666 ?
O2 Ni1 O1W 93.56(18) 13_666 . ?
O2 Ni1 O1W 86.44(18) 16_556 . ?
O2 Ni1 O1W 93.56(18) 4_665 . ?
O2 Ni1 O1W 86.45(18) . . ?
O1W Ni1 O1W 180.0 13_666 . ?
C1 O1 Eu1 126.2(4) . . ?
O2 C1 O1 126.0(6) . . ?
O2 C1 C2B 115.9(9) . . ?
O1 C1 C2B 117.5(8) . . ?
O2 C1 C2A 116.9(14) . . ?
O1 C1 C2A 114.9(14) . . ?
C1 O2 Ni1 130.8(5) . . ?
O3 C2A C1 107(2) . . ?
O3 C2A H2AA 110.4 . . ?
C1 C2A H2AA 110.4 . . ?
O3 C2A H2AB 110.4 . . ?
C1 C2A H2AB 110.4 . . ?
H2AA C2A H2AB 108.6 . . ?
O3 C2B C1 107.4(12) . . ?
O3 C2B H2BA 110.2 . . ?
C1 C2B H2BA 110.2 . . ?
O3 C2B H2BB 110.2 . . ?
C1 C2B H2BB 110.2 . . ?
H2BA C2B H2BB 108.5 . . ?
Ni1 O1W H1 108(6) . . ?
C2A O3 C2A 123(3) . 12 ?
C2A O3 C2B 112.1(12) . 12 ?
C2A O3 C2B 26.2(14) 12 12 ?
C2A O3 Eu1 118.4(15) . . ?
C2A O3 Eu1 118.4(15) 12 . ?
C2B O3 Eu1 123.2(7) . . ?
C2B O3 Eu1 123.2(7) 12 . ?

_refine_diff_density_max         1.195
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.141

_shelx_res_file                  
;
TITL cu_191127_LS_JT_EuNioda_0m_b.res in P6/mcc
    cu_191127_LS_JT_EuNioda_0m_b.res
    created by SHELXL-2018/3 at 19:22:56 on 23-Feb-2020
REM Old TITL cu_191127_LS_JT_EuNioda_0m in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.136,  Rweak 0.004,  Alpha 0.095,  Orientation as input
REM Formula found by SHELXT:  C24 Eu2 Ni3 O36
CELL  1.54178  14.5288  14.5288  15.6072   90.000   90.000  120.000
ZERR    2.000   0.0009   0.0009   0.0012    0.000    0.000    0.000
LATT  1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, Z
SYMM Y, -X+Y, Z
SYMM X-Y, X, Z
SYMM Y, X, 1/2-Z
SYMM X-Y, -Y, 1/2-Z
SYMM -X, -X+Y, 1/2-Z
SYMM -Y, -X, 1/2-Z
SYMM -X+Y, Y, 1/2-Z
SYMM X, X-Y, 1/2-Z
SFAC C H EU NI O
UNIT 48 72 4.0 6 81.12
TEMP 0
L.S. 10
BOND $H
ACTA
LIST 6
FMAP 2
PLAN 20
WGHT    0.088200    3.756300
EXTI    0.000822
FVAR       0.27941   0.35065
EU1   3    0.666667    0.333333    0.250000    10.16667    0.03602    0.03602 =
         0.02781    0.00000    0.00000    0.01801
NI1   4    0.500000    0.500000    0.500000    10.25000    0.03945    0.04359 =
         0.03440    0.00000    0.00000    0.02545
O1    5    0.579723    0.385766    0.355228    11.00000    0.05028    0.05973 =
         0.04451   -0.01228    0.00019    0.03025
C1    1    0.480586    0.351237    0.360828    11.00000    0.05118    0.05601 =
         0.05259   -0.01091   -0.00250    0.03060
O2    5    0.437751    0.384701    0.409258    11.00000    0.05036    0.07610 =
         0.06764   -0.02433   -0.00190    0.03543
PART 1
C2A   1    0.414729    0.284561    0.284006    21.00000    0.04712    0.05178 =
         0.06150   -0.01440    0.00771    0.02412
AFIX  23
H2AA  2    0.343706    0.232093    0.302312    21.00000   -1.20000
H2AB  2    0.409085    0.329820    0.241126    21.00000   -1.20000
AFIX   0
PART 2
C2B   1    0.406503    0.249650    0.312563   -21.00000    0.04423    0.05031 =
         0.06086   -0.00891    0.00400    0.02111
AFIX  23
H2BA  2    0.374796    0.189824    0.351726   -21.00000   -1.20000
H2BB  2    0.350002    0.256103    0.285282   -21.00000   -1.20000
AFIX   0
PART 0
SIMU 0.01 0.02 2.0 C2A C2B
O1W   5    0.352738    0.493238    0.500000    10.50000    0.04912    0.05376 =
         0.04121    0.00000    0.00000    0.03229
O3    5    0.468156    0.234078    0.250000    10.50000    0.04081    0.05357 =
         0.04803   -0.01627    0.00000    0.02041
H1    2    0.352893    0.536754    0.457081    11.00000    0.09776
O2W   5    0.207201    0.235979    0.500000    10.38000    0.35459
REM #####
HKLF 4




REM  cu_191127_LS_JT_EuNioda_0m_b.res in P6/mcc
REM wR2 = 0.1576, GooF = S = 1.133, Restrained GooF = 1.130 for all data
REM R1 = 0.0553 for 823 Fo > 4sig(Fo) and 0.0685 for all 1043 data
REM 72 parameters refined using 6 restraints

END

WGHT      0.0882      3.7565

REM Highest difference peak  1.195,  deepest hole -0.498,  1-sigma level  0.141
Q1    1   0.0000  0.0000  0.2500  10.08333  0.05    1.20
Q2    1   0.1003  0.1532  0.6382  11.00000  0.05    0.69
Q3    1   0.2320  0.2066  0.5000  10.50000  0.05    0.61
Q4    1   0.1677  0.3305  0.5000  10.50000  0.05    0.60
Q5    1   0.1516  0.0758  0.2500  10.50000  0.05    0.48
Q6    1   0.7159  0.4318  0.2500  10.50000  0.05    0.46
Q7    1   0.1807  0.2737  0.5000  10.50000  0.05    0.45
Q8    1   0.7573  0.4132  0.2525  11.00000  0.05    0.43
Q9    1   0.1502  0.1104  0.2470  11.00000  0.05    0.41
Q10   1   0.4022  0.4612  0.5000  10.50000  0.05    0.39
Q11   1   0.6667  0.3333  0.1603  10.33333  0.05    0.37
Q12   1   0.2078  0.1039  0.2500  10.50000  0.05    0.37
Q13   1   0.5498  0.6041  0.5000  10.50000  0.05    0.36
Q14   1   0.2007  0.2553  0.4548  11.00000  0.05    0.34
Q15   1   0.6233  0.2364  0.2222  11.00000  0.05    0.32
Q16   1   0.2333  0.2540  0.4162  11.00000  0.05    0.31
Q17   1   0.0000  0.0000  0.5000  10.08333  0.05    0.28
Q18   1   0.3301  0.4159  0.5000  10.50000  0.05    0.26
Q19   1   0.5000  0.5000  0.4175  10.50000  0.05    0.25
Q20   1   0.6297  0.4217  0.3598  11.00000  0.05    0.24
;
_shelx_res_checksum              59135

_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_preparation       'proton conductor'
####################################################################### 
# 
# 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_Y-Ni
_database_code_depnum_ccdc_archive 'CCDC 1987750'
loop_
_audit_author_name
_audit_author_address
'Leopoldo Suescun'
;Facultad de Quimica, Universidad de la Republica, Uruguay
Uruguay
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_Y-Ni                
;
PROBLEM: Short Inter D-H..H-D       H1       ..H1       .       1.42 Ang.  
RESPONSE: This is not an intermolecular H-H distance but intramolecular in
a water molecule placed over a mirror plane.
;
_vrf_PLAT601_Y-Ni                
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        364 Ang**3
RESPONSE: This compound is a MOF with large voids occupied by disordered 
solvent molecules that were partially modelled.
;
_vrf_PLAT202_Y-Ni                
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check 
RESPONSE: These corresponds to the solvent molecules (O2W) filling 
the MOF's voids, which could only be modelled isotropically due to its 
high disorder.
;
_vrf_PLAT241_Y-Ni                
;
PROBLEM: High   MainMol Ueq as Compared to Neighbors of         O2 Check   
RESPONSE: The oxidiacetate ligand possesses a slight disorder that 
enhances the Ueq of the light elements in comparison to that of Ni atoms, 
which lie in special positions. Such disorder is not enough to justify a 
splitting in the case of O2, but it is enough to generate an appreciable 
difference of U against Ni.
;
_vrf_PLAT242_Y-Ni                
;
PROBLEM: Low    MainMol Ueq as Compared to Neighbors of        Ni1 Check   
RESPONSE: The oxidiacetate ligand possesses a slight disorder that 
enhances the Ueq of the light elements in comparison to that of Ni atoms, 
which lie in special positions. Such disorder is not enough to justify a 
splitting in the case of O2, but it is enough to generate an appreciable 
difference of U against Ni.
;
_vrf_PLAT314_Y-Ni                
;
PROBLEM: Small Angle for H2O: Metal-O4       -H1        .      89.90 Degree
RESPONSE: It is rather difficult to model water H atoms in this compound 
due to the presence of heavy atoms and strong disorder of water molecules.
The refined position of H1 is the best that could be attained with the
available data. The position is not at all imporobable since H1 forms an 
H-bond with O1 that may justify the observation of the small Ni-O4-H1 angle.
;
_vrf_PLAT906_Y-Ni                
;
PROBLEM: Large K Value in the Analysis of Variance ......      4.914 Check 
RESPONSE: It is a frequent problem of area detectors to overestimate the
background and let some low intensity reflections underestimated. For this
reason, for a small number of low intensity reflections below 1% of Fcmax
a rather large K value is found.
;
# end Validation Reply Form

_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            'C24 H36 Ni3 O40.20 Y2'
_chemical_formula_weight         1321.68

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'
Ni Ni -3.0029 0.5091 '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'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   13.9318(10)
_cell_length_b                   13.9318(10)
_cell_length_c                   16.1061(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2707.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1056
_cell_measurement_theta_min      4.22
_cell_measurement_theta_max      22.16

_exptl_crystal_description       'hexagonal needle'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_F_000             1327
_exptl_transmission_factor_min   0.058243
_exptl_transmission_factor_max   0.178492
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.823
_shelx_estimated_absorpt_T_min   0.484
_shelx_estimated_absorpt_T_max   0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 10.83333
_diffrn_reflns_number            2712
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.663
_diffrn_reflns_theta_max         86.415
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2712
_reflns_number_gt                2360
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 3-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1358P)²+0.6391P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2712
_refine_ls_number_parameters     75
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.2050
_refine_ls_wR_factor_gt          0.1937
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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
Y1 Y 0.666667 0.333333 0.750000 0.0446(4) Uani 1 6 d S T P A .
H1WW H 0.626(5) 0.173(5) 0.544(4) 0.084(16) Uiso 1 1 d . . . . .
C2A C 0.4029(15) 0.1602(18) 0.6833(14) 0.063(3) Uani 0.61(5) 1 d . U P A 1
H2AA H 0.376814 0.196918 0.645986 0.076 Uiso 0.61(5) 1 calc R U P A 1
H2AB H 0.339196 0.094002 0.705020 0.076 Uiso 0.61(5) 1 calc R U P A 1
C2B C 0.410(3) 0.135(3) 0.707(2) 0.070(6) Uani 0.39(5) 1 d . U P A 2
H2BA H 0.342465 0.127464 0.684128 0.084 Uiso 0.39(5) 1 calc R U P A 2
H2BB H 0.390557 0.073322 0.744355 0.084 Uiso 0.39(5) 1 calc R U P A 2
Ni1 Ni 0.500000 0.000000 0.500000 0.0455(5) Uani 1 4 d S T P . .
O1 O 0.5810(2) 0.1946(3) 0.6470(2) 0.0588(8) Uani 1 1 d . . . . .
O2 O 0.4349(2) 0.0538(3) 0.5882(2) 0.0692(9) Uani 1 1 d . . . . .
O3 O 0.4663(4) 0.2332(2) 0.750000 0.0565(11) Uani 1 2 d S T P . .
C1 C 0.4791(3) 0.1306(4) 0.6384(3) 0.0579(10) Uani 1 1 d . . . . .
O1W O 0.6514(3) 0.1462(3) 0.500000 0.0546(9) Uani 1 2 d S T P . .
O2W O 0.798(3) 0.0099(19) 0.500000 0.259(13) Uiso 0.7 2 d S . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.0493(5) 0.0493(5) 0.0354(6) 0.000 0.000 0.0246(2)
C2A 0.061(4) 0.069(8) 0.060(8) -0.015(6) -0.004(5) 0.032(5)
C2B 0.065(8) 0.067(12) 0.063(13) -0.028(9) -0.003(9) 0.023(8)
Ni1 0.0501(7) 0.0420(7) 0.0396(8) 0.000 0.000 0.0195(5)
O1 0.0576(15) 0.0595(17) 0.0534(16) -0.0120(14) -0.0005(12) 0.0247(13)
O2 0.0610(17) 0.0666(18) 0.069(2) -0.0233(15) 0.0022(13) 0.0236(14)
O3 0.053(2) 0.0615(19) 0.052(2) -0.0132(13) 0.000 0.0265(11)
C1 0.060(2) 0.057(2) 0.054(2) -0.0069(17) -0.0004(17) 0.0267(19)
O1W 0.057(2) 0.050(2) 0.051(2) 0.000 0.000 0.0223(17)

_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
Y1 O1 2.368(3) 12_556 ?
Y1 O1 2.368(3) 3_665 ?
Y1 O1 2.368(3) . ?
Y1 O1 2.368(3) 10_666 ?
Y1 O1 2.368(3) 11_656 ?
Y1 O1 2.368(3) 2_655 ?
Y1 O3 2.417(5) 2_655 ?
Y1 O3 2.417(5) 3_665 ?
Y1 O3 2.417(5) . ?
C2A O3 1.439(19) . ?
C2A C1 1.503(19) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2B O3 1.38(3) . ?
C2B C1 1.48(3) . ?
C2B H2BA 0.9700 . ?
C2B H2BB 0.9700 . ?
Ni1 O2 2.021(3) . ?
Ni1 O2 2.021(3) 16_556 ?
Ni1 O2 2.021(3) 4_655 ?
Ni1 O2 2.021(3) 13_656 ?
Ni1 O1W 2.073(4) 13_656 ?
Ni1 O1W 2.073(4) . ?
O1 C1 1.250(5) . ?
O2 C1 1.233(5) . ?
O1W H1WW 0.95(6) . ?

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 Y1 O1 90.02(18) 12_556 3_665 ?
O1 Y1 O1 128.25(15) 12_556 . ?
O1 Y1 O1 76.32(13) 3_665 . ?
O1 Y1 O1 76.32(13) 12_556 10_666 ?
O1 Y1 O1 128.25(15) 3_665 10_666 ?
O1 Y1 O1 148.60(16) . 10_666 ?
O1 Y1 O1 76.32(13) 12_556 11_656 ?
O1 Y1 O1 148.60(16) 3_665 11_656 ?
O1 Y1 O1 90.02(18) . 11_656 ?
O1 Y1 O1 76.32(13) 10_666 11_656 ?
O1 Y1 O1 148.60(16) 12_556 2_655 ?
O1 Y1 O1 76.32(13) 3_665 2_655 ?
O1 Y1 O1 76.32(13) . 2_655 ?
O1 Y1 O1 90.02(18) 10_666 2_655 ?
O1 Y1 O1 128.25(15) 11_656 2_655 ?
O1 Y1 O3 134.99(9) 12_556 2_655 ?
O1 Y1 O3 134.99(9) 3_665 2_655 ?
O1 Y1 O3 74.30(8) . 2_655 ?
O1 Y1 O3 74.30(8) 10_666 2_655 ?
O1 Y1 O3 64.12(7) 11_656 2_655 ?
O1 Y1 O3 64.12(7) 2_655 2_655 ?
O1 Y1 O3 74.30(8) 12_556 3_665 ?
O1 Y1 O3 64.13(7) 3_665 3_665 ?
O1 Y1 O3 134.99(9) . 3_665 ?
O1 Y1 O3 64.13(7) 10_666 3_665 ?
O1 Y1 O3 134.99(9) 11_656 3_665 ?
O1 Y1 O3 74.30(8) 2_655 3_665 ?
O3 Y1 O3 120.000(1) 2_655 3_665 ?
O1 Y1 O3 64.13(7) 12_556 . ?
O1 Y1 O3 74.30(8) 3_665 . ?
O1 Y1 O3 64.13(7) . . ?
O1 Y1 O3 134.99(9) 10_666 . ?
O1 Y1 O3 74.30(8) 11_656 . ?
O1 Y1 O3 134.99(9) 2_655 . ?
O3 Y1 O3 120.0 2_655 . ?
O3 Y1 O3 120.0 3_665 . ?
O3 C2A C1 106.5(11) . . ?
O3 C2A H2AA 110.4 . . ?
C1 C2A H2AA 110.4 . . ?
O3 C2A H2AB 110.4 . . ?
C1 C2A H2AB 110.4 . . ?
H2AA C2A H2AB 108.6 . . ?
O3 C2B C1 111.1(19) . . ?
O3 C2B H2BA 109.4 . . ?
C1 C2B H2BA 109.4 . . ?
O3 C2B H2BB 109.4 . . ?
C1 C2B H2BB 109.4 . . ?
H2BA C2B H2BB 108.0 . . ?
O2 Ni1 O2 89.4(2) . 16_556 ?
O2 Ni1 O2 90.6(2) . 4_655 ?
O2 Ni1 O2 180.00(14) 16_556 4_655 ?
O2 Ni1 O2 180.0 . 13_656 ?
O2 Ni1 O2 90.6(2) 16_556 13_656 ?
O2 Ni1 O2 89.4(2) 4_655 13_656 ?
O2 Ni1 O1W 86.53(12) . 13_656 ?
O2 Ni1 O1W 86.53(12) 16_556 13_656 ?
O2 Ni1 O1W 93.47(12) 4_655 13_656 ?
O2 Ni1 O1W 93.47(12) 13_656 13_656 ?
O2 Ni1 O1W 93.47(12) . . ?
O2 Ni1 O1W 93.47(12) 16_556 . ?
O2 Ni1 O1W 86.53(12) 4_655 . ?
O2 Ni1 O1W 86.53(12) 13_656 . ?
O1W Ni1 O1W 180.0 13_656 . ?
C1 O1 Y1 126.0(3) . . ?
C1 O2 Ni1 131.4(3) . . ?
C2B O3 C2B 121(3) 12_556 . ?
C2A O3 C2A 115.7(16) . 12_556 ?
C2B O3 Y1 119.3(15) 12_556 . ?
C2B O3 Y1 119.3(14) . . ?
C2A O3 Y1 122.2(8) . . ?
C2A O3 Y1 122.2(8) 12_556 . ?
O2 C1 O1 126.0(4) . . ?
O2 C1 C2B 118.0(11) . . ?
O1 C1 C2B 114.7(12) . . ?
O2 C1 C2A 116.0(8) . . ?
O1 C1 C2A 117.3(8) . . ?
Ni1 O1W H1WW 90(4) . . ?

_refine_diff_density_max         0.817
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.164

_shelx_res_file                  
;
TITL cu_191101_GP_JT_YNioda_0m_4_a.res in P6/mcc
    Y-Ni.res
    created by SHELXL-2018/3 at 18:47:17 on 23-Feb-2020
REM Old TITL cu_191101_GP_JT_YNioda_0m_4 in P6/mcc
REM SHELXT solution in P6/mcc
REM R1 0.136,  Rweak 0.001,  Alpha 0.034,  Orientation as input
REM Formula found by SHELXT:  C24 Ni3 O36 Y2
CELL  1.54178  13.9318  13.9318  16.1061   90.000   90.000  120.000
ZERR    2.000   0.0010   0.0010   0.0013    0.000    0.000    0.000
LATT  1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, Z
SYMM Y, -X+Y, Z
SYMM X-Y, X, Z
SYMM Y, X, 1/2-Z
SYMM X-Y, -Y, 1/2-Z
SYMM -X, -X+Y, 1/2-Z
SYMM -Y, -X, 1/2-Z
SYMM -X+Y, Y, 1/2-Z
SYMM X, X-Y, 1/2-Z
SFAC C H NI O Y
UNIT 48 72 6 80.4 4.00008
TEMP 0
SIZE 0.05 0.094 0.176
L.S. 10
BOND $H
ACTA
LIST 6
FMAP 2
PLAN 20
WGHT    0.135800    0.639100
SWAT    3.745795   16.7860
BASF   0.21799   0.37610
FVAR       0.45797   0.60579
Y1    5    0.666667    0.333333    0.750000    10.16666    0.04926    0.04926 =
         0.03538    0.00000    0.00000    0.02463
H1WW  2    0.626284    0.172833    0.544049    11.00000    0.08405
PART 1
C2A   1    0.402851    0.160152    0.683299    21.00000    0.06063    0.06919 =
         0.05950   -0.01529   -0.00353    0.03172
AFIX  23
H2AA  2    0.376814    0.196918    0.645986    21.00000   -1.20000
H2AB  2    0.339196    0.094002    0.705020    21.00000   -1.20000
AFIX   0
PART 2
C2B   1    0.410358    0.134857    0.706776   -21.00000    0.06513    0.06719 =
         0.06281   -0.02765   -0.00288    0.02251
AFIX  23
H2BA  2    0.342465    0.127464    0.684128   -21.00000   -1.20000
H2BB  2    0.390557    0.073322    0.744355   -21.00000   -1.20000
AFIX   0
PART 0
SIMU 0.01 0.02 2.0 C2A C2B
NI1   3    0.500000    0.000000    0.500000    10.25000    0.05009    0.04201 =
         0.03962    0.00000    0.00000    0.01954
O1    4    0.581014    0.194568    0.646974    11.00000    0.05755    0.05950 =
         0.05337   -0.01197   -0.00046    0.02475
O2    4    0.434869    0.053826    0.588239    11.00000    0.06100    0.06661 =
         0.06890   -0.02333    0.00220    0.02365
O3    4    0.466337    0.233169    0.750000    10.50000    0.05309    0.06148 =
         0.05206   -0.01317    0.00000    0.02654
C1    1    0.479134    0.130630    0.638447    11.00000    0.05959    0.05676 =
         0.05426   -0.00687   -0.00036    0.02673
O1W   4    0.651370    0.146157    0.500000    10.50000    0.05702    0.05011 =
         0.05059    0.00000    0.00000    0.02230
O2W   4    0.798378    0.009858    0.500000    10.35000    0.25949
REM #####
HKLF 5




REM  cu_191101_GP_JT_YNioda_0m_4_a.res in P6/mcc
REM wR2 = 0.2050, GooF = S = 1.084, Restrained GooF = 1.084 for all data
REM R1 = 0.0653 for 2360 Fo > 4sig(Fo) and 0.0748 for all 2712 data
REM 75 parameters refined using 6 restraints

END

WGHT      0.1382      0.6436

REM Highest difference peak  0.817,  deepest hole -0.867,  1-sigma level  0.164
Q1    1   0.1190 -0.0165  0.6800  11.00000  0.05    0.82
Q2    1   0.7980  0.0185  0.5492  11.00000  0.05    0.73
Q3    1   0.8151  0.0690  0.4660  11.00000  0.05    0.58
Q4    1   0.0000  0.0000  0.7500  10.08333  0.05    0.42
Q5    1   1.0000  0.0000  0.3189  10.16667  0.05    0.30
Q6    1   0.8385 -0.0484  0.4201  11.00000  0.05    0.28
Q7    1   0.3313  0.0229  0.5852  11.00000  0.05    0.17
Q8    1   0.6162  0.2310  0.7674  11.00000  0.05    0.16
Q9    1   0.2467  0.0582  0.6767  11.00000  0.05    0.12
Q10   1   0.3496  0.0473  0.5360  11.00000  0.05    0.11
Q11   1   0.7002 -0.0253  0.5365  11.00000  0.05    0.10
Q12   1   0.7324  0.3007  0.5345  11.00000  0.05    0.10
Q13   1   0.3631 -0.0582  0.5876  11.00000  0.05    0.10
Q14   1   0.7105  0.2381  0.5320  11.00000  0.05    0.09
Q15   1   0.5971  0.1081  0.6706  11.00000  0.05    0.09
Q16   1   0.5397  0.2015  0.7591  11.00000  0.05    0.09
Q17   1   0.3237  0.0000  0.7500  10.50000  0.05    0.09
Q18   1   0.3837  0.0090  0.7798  11.00000  0.05    0.08
Q19   1   0.5615  0.2808  0.7500  10.50000  0.05    0.08
Q20   1   0.3744  0.2234  0.6947  11.00000  0.05    0.08
;
_shelx_res_checksum              41599

_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_preparation       'proton conductor'
####################################################################### 
# 
# 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_mo_180609_FI_CeNioda_final_OK
_database_code_depnum_ccdc_archive 'CCDC 1987751'
loop_
_audit_author_name
_audit_author_address
'Leopoldo Suescun'
;Facultad de Quimica, Universidad de la Republica, Uruguay
Uruguay
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_mo_180609_FI_CeNioda_final_OK 
;
PROBLEM: Short Inter D-H..H-D       H1W      ..H1W      .       1.33 Ang.  
RESPONSE: This is not an intermolecular H-H distance but intramolecular in
a water molecule placed over a mirror plane.
;
_vrf_PLAT601_mo_180609_FI_CeNioda_final_OK 
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        489 Ang**3
RESPONSE: This compound is a MOF with large voids occupied by disordered 
solvent molecules that were partially modelled.
;
_vrf_PLAT202_mo_180609_FI_CeNioda_final_OK 
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check 
RESPONSE: These corresponds to the solvent molecules (O2WA and O2WB) filling 
the MOF's voids, which could only be modelled isotropically due to their 
large disorder.
;
_vrf_PLAT250_mo_180609_FI_CeNioda_final_OK 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note  
RESPONSE: Multi-scan absorption correction did not manage to correct this due to 
the highly anisotropic crystal shape.
;
_vrf_PLAT911_mo_180609_FI_CeNioda_final_OK 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.595          2 Report
RESPONSE: These correspond to the 004 and 008 reflections. The 004 
reflection saturates the detector on both the full collection and 
the fast scan. The 008 reflection is not included in the integration 
by the software algorithm.
;
_vrf_PLAT918_mo_180609_FI_CeNioda_final_OK 
;
PROBLEM: Reflection(s) with I(obs) much Smaller I(calc) .          4 Check 
RESPONSE: The discrepancy arises on the partially modelled solvent.
;
_vrf_PLAT939_mo_180609_FI_CeNioda_final_OK 
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .      22.00 Check 
RESPONSE: Large weight values are a result of missing and unmatching reflections
previously explained.
;
# end Validation Reply Form
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H36 Ce2 Ni3 O42'
_chemical_formula_weight         1452.90

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_H-M_alt        'P 6/m c c'
_space_group_name_Hall           '-P 6 2c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   15.0898(7)
_cell_length_b                   15.0898(7)
_cell_length_c                   15.1899(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2995.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    956
_cell_measurement_theta_min      3.568
_cell_measurement_theta_max      23.54

_exptl_crystal_description       'hexagonal needle'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.126
_exptl_absorpt_coefficient_mu    2.509
_shelx_estimated_absorpt_T_min   0.432
_shelx_estimated_absorpt_T_max   0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6099
_exptl_absorpt_correction_T_max  0.7482
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 10.83333
_diffrn_reflns_number            38785
_diffrn_reflns_av_unetI/netI     0.0066
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.102
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_full        25.020
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             923
_reflns_number_gt                890
_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.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0763P)²+2.9485P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         923
_refine_ls_number_parameters     83
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.1116
_refine_ls_wR_factor_gt          0.1108
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.000
_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
Ce1 Ce 0.6667 0.3333 0.2500 0.0178(3) Uani 1 6 d S T P A .
O1 O 0.80710(17) 0.38212(19) 0.35778(15) 0.0332(5) Uani 1 1 d D U . . .
C1A C 0.8710(2) 0.3522(2) 0.35974(19) 0.0324(6) Uani 0.51(2) 1 d . U P A 1
O2A O 0.9417(7) 0.3789(7) 0.4155(6) 0.0329(15) Uani 0.51(2) 1 d D U P A 1
C2A C 0.8423(8) 0.2519(7) 0.3144(8) 0.0313(14) Uani 0.51(2) 1 d D U P A 1
H2A1 H 0.9017 0.2558 0.2860 0.038 Uiso 0.51(2) 1 calc R U P A 1
H2A2 H 0.8158 0.1965 0.3568 0.038 Uiso 0.51(2) 1 calc R U P A 1
C1B C 0.8710(2) 0.3522(2) 0.35974(19) 0.0324(6) Uani 0.49(2) 1 d . U P A 2
O2B O 0.9565(6) 0.3977(8) 0.3976(6) 0.0316(15) Uani 0.49(2) 1 d D U P A 2
C2B C 0.8639(7) 0.2787(9) 0.2874(8) 0.0333(15) Uani 0.49(2) 1 d D U P A 2
H2B1 H 0.9155 0.3154 0.2428 0.040 Uiso 0.49(2) 1 calc R U P A 2
H2B2 H 0.8750 0.2257 0.3118 0.040 Uiso 0.49(2) 1 calc R U P A 2
Ni1 Ni 1.0000 0.5000 0.5000 0.0190(3) Uani 1 4 d S T P . .
O3 O 0.76513(13) 0.23487(13) 0.2500 0.0313(8) Uani 1 2 d S T P . .
O1W O 0.8660(2) 0.5090(2) 0.5000 0.0264(6) Uani 1 2 d DS T P A .
H1W H 0.840(2) 0.4717(14) 0.4562(3) 0.039(9) Uiso 1 1 d D . . . .
O2WA O 1.066(2) 0.267(2) 0.5000 0.239(9) Uiso 0.63(2) 2 d S U P B 1
O2WB O 0.969(4) 0.209(4) 0.5000 0.239(9) Uiso 0.37(2) 2 d S U P B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ce1 0.0194(3) 0.0194(3) 0.0147(4) 0.000 0.000 0.00969(14)
O1 0.0320(11) 0.0406(11) 0.0326(11) -0.0150(10) -0.0144(9) 0.0224(10)
C1A 0.0275(12) 0.0374(13) 0.0340(13) -0.0125(10) -0.0116(10) 0.0175(10)
O2A 0.029(2) 0.037(3) 0.034(3) -0.012(2) -0.014(2) 0.0172(19)
C2A 0.028(3) 0.035(3) 0.034(3) -0.012(2) -0.014(2) 0.018(2)
C1B 0.0275(12) 0.0374(13) 0.0340(13) -0.0125(10) -0.0116(10) 0.0175(10)
O2B 0.025(2) 0.041(3) 0.030(3) -0.014(2) -0.010(2) 0.017(2)
C2B 0.026(3) 0.039(3) 0.037(3) -0.014(2) -0.013(2) 0.018(2)
Ni1 0.0156(5) 0.0219(4) 0.0167(5) 0.000 0.000 0.0072(3)
O3 0.0306(13) 0.0306(13) 0.0372(18) -0.0167(9) -0.0167(9) 0.0187(16)
O1W 0.0231(13) 0.0303(14) 0.0246(14) 0.000 0.000 0.0124(12)

_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
Ce1 O1 2.480(2) 10_665 ?
Ce1 O1 2.480(2) 12 ?
Ce1 O1 2.480(2) 3_665 ?
Ce1 O1 2.480(2) 11_655 ?
Ce1 O1 2.480(2) 2_655 ?
Ce1 O1 2.481(2) . ?
Ce1 O3 2.573(4) 3_665 ?
Ce1 O3 2.573(4) 2_655 ?
Ce1 O3 2.573(4) . ?
O1 C1B 1.253(4) . ?
O1 C1A 1.253(4) . ?
C1A O2A 1.260(8) . ?
C1A C2A 1.515(7) . ?
O2A Ni1 2.038(8) . ?
C2A O3 1.443(8) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C1B O2B 1.257(8) . ?
C1B C2B 1.526(8) . ?
O2B Ni1 2.055(9) . ?
C2B O3 1.412(8) . ?
C2B H2B1 0.9700 . ?
C2B H2B2 0.9700 . ?
Ni1 O2A 2.038(9) 13_766 ?
Ni1 O2A 2.038(9) 16_556 ?
Ni1 O2A 2.038(9) 4_765 ?
Ni1 O2B 2.055(9) 13_766 ?
Ni1 O2B 2.055(9) 16_556 ?
Ni1 O2B 2.055(9) 4_765 ?
Ni1 O1W 2.094(3) 13_766 ?
Ni1 O1W 2.094(3) . ?
O3 C2B 1.412(8) 10_665 ?
O3 C2A 1.443(8) 10_665 ?
O1W H1W 0.832(9) . ?

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 Ce1 O1 81.17(8) 10_665 12 ?
O1 Ce1 O1 84.56(11) 10_665 3_665 ?
O1 Ce1 O1 150.21(11) 12 3_665 ?
O1 Ce1 O1 81.17(8) 10_665 11_655 ?
O1 Ce1 O1 81.17(8) 12 11_655 ?
O1 Ce1 O1 122.26(10) 3_665 11_655 ?
O1 Ce1 O1 150.21(11) 10_665 2_655 ?
O1 Ce1 O1 122.26(10) 12 2_655 ?
O1 Ce1 O1 81.17(8) 3_665 2_655 ?
O1 Ce1 O1 84.56(11) 11_655 2_655 ?
O1 Ce1 O1 122.26(10) 10_665 . ?
O1 Ce1 O1 84.56(11) 12 . ?
O1 Ce1 O1 81.17(8) 3_665 . ?
O1 Ce1 O1 150.21(11) 11_655 . ?
O1 Ce1 O1 81.17(8) 2_655 . ?
O1 Ce1 O3 75.10(6) 10_665 3_665 ?
O1 Ce1 O3 137.72(6) 12 3_665 ?
O1 Ce1 O3 61.13(5) 3_665 3_665 ?
O1 Ce1 O3 61.13(5) 11_655 3_665 ?
O1 Ce1 O3 75.11(6) 2_655 3_665 ?
O1 Ce1 O3 137.72(6) . 3_665 ?
O1 Ce1 O3 137.72(6) 10_665 2_655 ?
O1 Ce1 O3 61.13(5) 12 2_655 ?
O1 Ce1 O3 137.72(6) 3_665 2_655 ?
O1 Ce1 O3 75.11(6) 11_655 2_655 ?
O1 Ce1 O3 61.13(5) 2_655 2_655 ?
O1 Ce1 O3 75.10(6) . 2_655 ?
O3 Ce1 O3 120.0 3_665 2_655 ?
O1 Ce1 O3 61.13(5) 10_665 . ?
O1 Ce1 O3 75.10(6) 12 . ?
O1 Ce1 O3 75.10(6) 3_665 . ?
O1 Ce1 O3 137.72(6) 11_655 . ?
O1 Ce1 O3 137.72(6) 2_655 . ?
O1 Ce1 O3 61.13(5) . . ?
O3 Ce1 O3 120.0 3_665 . ?
O3 Ce1 O3 120.0 2_655 . ?
C1B O1 Ce1 127.30(18) . . ?
C1A O1 Ce1 127.30(18) . . ?
O1 C1A O2A 125.6(5) . . ?
O1 C1A C2A 117.5(4) . . ?
O2A C1A C2A 113.5(6) . . ?
C1A O2A Ni1 128.8(7) . . ?
O3 C2A C1A 106.7(5) . . ?
O3 C2A H2A1 110.4 . . ?
C1A C2A H2A1 110.4 . . ?
O3 C2A H2A2 110.4 . . ?
C1A C2A H2A2 110.4 . . ?
H2A1 C2A H2A2 108.6 . . ?
O1 C1B O2B 125.4(5) . . ?
O1 C1B C2B 117.2(4) . . ?
O2B C1B C2B 113.9(6) . . ?
C1B O2B Ni1 127.7(7) . . ?
O3 C2B C1B 107.7(5) . . ?
O3 C2B H2B1 110.2 . . ?
C1B C2B H2B1 110.2 . . ?
O3 C2B H2B2 110.2 . . ?
C1B C2B H2B2 110.2 . . ?
H2B1 C2B H2B2 108.5 . . ?
O2A Ni1 O2A 180.0 . 13_766 ?
O2A Ni1 O2A 78.1(6) . 16_556 ?
O2A Ni1 O2A 101.9(6) 13_766 16_556 ?
O2A Ni1 O2A 101.9(6) . 4_765 ?
O2A Ni1 O2A 78.1(6) 13_766 4_765 ?
O2A Ni1 O2A 180.0(5) 16_556 4_765 ?
O2B Ni1 O2B 81.6(6) 13_766 16_556 ?
O2B Ni1 O2B 98.4(6) 13_766 4_765 ?
O2B Ni1 O2B 180.0(5) 16_556 4_765 ?
O2B Ni1 O2B 180.0 13_766 . ?
O2B Ni1 O2B 98.4(6) 16_556 . ?
O2B Ni1 O2B 81.6(6) 4_765 . ?
O2A Ni1 O1W 86.6(3) . 13_766 ?
O2A Ni1 O1W 93.4(3) 13_766 13_766 ?
O2A Ni1 O1W 86.6(3) 16_556 13_766 ?
O2A Ni1 O1W 93.4(3) 4_765 13_766 ?
O2B Ni1 O1W 95.3(2) 13_766 13_766 ?
O2B Ni1 O1W 84.7(2) 16_556 13_766 ?
O2B Ni1 O1W 95.3(2) 4_765 13_766 ?
O2B Ni1 O1W 84.7(2) . 13_766 ?
O2A Ni1 O1W 93.4(3) . . ?
O2A Ni1 O1W 86.6(3) 13_766 . ?
O2A Ni1 O1W 93.4(3) 16_556 . ?
O2A Ni1 O1W 86.6(3) 4_765 . ?
O2B Ni1 O1W 84.7(2) 13_766 . ?
O2B Ni1 O1W 95.3(2) 16_556 . ?
O2B Ni1 O1W 84.7(2) 4_765 . ?
O2B Ni1 O1W 95.3(2) . . ?
O1W Ni1 O1W 180.0 13_766 . ?
C2B O3 C2B 119.0(7) 10_665 . ?
C2A O3 C2A 114.0(6) 10_665 . ?
C2B O3 Ce1 120.5(4) 10_665 . ?
C2B O3 Ce1 120.5(4) . . ?
C2A O3 Ce1 123.0(3) 10_665 . ?
C2A O3 Ce1 123.0(3) . . ?
Ni1 O1W H1W 96(2) . . ?

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
O1W H1W O1 0.832(9) 1.907(12) 2.724(3) 167(3) .

_refine_diff_density_max         0.622
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.112

_shelx_res_file                  
;

    mo_180609_FI_CeNioda_final_OK.res created by SHELXL-2014/7


TITL mo_180609_FI_CeNioda_0m_a.res in P6/mcc
REM Old TITL mo_180609_FI_CeNioda_0m in P6/mcc

REM SHELXT solution in P6/mcc
REM R1 0.121,  Rweak 0.000,  Alpha 0.042,  Orientation as input
REM Formula found by SHELXT:  C24 O36 Ni3 Ce2

CELL  0.71073  15.0898  15.0898  15.1899   90.000   90.000  120.000
ZERR    2.000   0.0007   0.0007   0.0007    0.000    0.000    0.000
LATT  1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, Z
SYMM Y, -X+Y, Z
SYMM X-Y, X, Z
SYMM Y, X, 1/2-Z
SYMM X-Y, -Y, 1/2-Z
SYMM -X, -X+Y, 1/2-Z
SYMM -Y, -X, 1/2-Z
SYMM -X+Y, Y, 1/2-Z
SYMM X, X-Y, 1/2-Z
SFAC C H O NI CE
UNIT 48 72 84 6 4.00008
EQIV $1 X, Y, 1-Z
TEMP 25
HTAB O1W O1
L.S. 100
ACTA
SIZE 0.126 0.233 0.402
BOND $H
LIST 6
FMAP 2
PLAN 20
WGHT    0.076300    2.948500
FVAR       0.30440   0.50535   0.62606   0.23935
CE1   5    0.666667    0.333333    0.250000    10.16667    0.01938    0.01938 =
         0.01470    0.00000    0.00000    0.00969
SAME 0.01 O1 C1A O2B C2B
SIMU 0.005 O1 > C2B
O1    3    0.807099    0.382125    0.357783    11.00000    0.03205    0.04062 =
         0.03256   -0.01496   -0.01440    0.02239
PART 1 21
C1A   1    0.871012    0.352209    0.359744    21.00000    0.02747    0.03741 =
         0.03403   -0.01245   -0.01157    0.01753
O2A   3    0.941657    0.378893    0.415498    21.00000    0.02875    0.03685 =
         0.03413   -0.01193   -0.01362    0.01724
C2A   1    0.842340    0.251929    0.314415    21.00000    0.02823    0.03519 =
         0.03396   -0.01211   -0.01384    0.01848
AFIX  23
H2A1  2    0.901740    0.255818    0.285973    21.00000   -1.20000
H2A2  2    0.815772    0.196469    0.356841    21.00000   -1.20000
AFIX   0
PART 2 -21
EXYZ C1A C1B
EADP C1A C1B
C1B   1    0.871012    0.352209    0.359744   -21.00000    0.02747    0.03741 =
         0.03403   -0.01245   -0.01157    0.01753
O2B   3    0.956534    0.397671    0.397567   -21.00000    0.02458    0.04053 =
         0.03021   -0.01377   -0.00986    0.01671
C2B   1    0.863880    0.278744    0.287372   -21.00000    0.02642    0.03861 =
         0.03702   -0.01386   -0.01279    0.01797
AFIX  23
H2B1  2    0.915493    0.315355    0.242751   -21.00000   -1.20000
H2B2  2    0.875007    0.225721    0.311844   -21.00000   -1.20000
AFIX   0
PART 0
NI1   4    1.000000    0.500000    0.500000    10.25000    0.01557    0.02189 =
         0.01670    0.00000    0.00000    0.00715
O3    3    0.765126    0.234874    0.250000    10.50000    0.03062    0.03062 =
         0.03723   -0.01672   -0.01672    0.01868
DFIX 0.83 0.01 O1W H1W
DANG 1.33 0.01 H1W H1W_$1
O1W   3    0.865957    0.508960    0.500000    10.50000    0.02306    0.03031 =
         0.02459    0.00000    0.00000    0.01236
H1W   2    0.839974    0.471737    0.456170    11.00000    0.03934
PART 1
O2WA  3    1.065823    0.267105    0.500000    30.50000   41.00000
PART 2
O2WB  3    0.969043    0.208737    0.500000   -30.50000   41.00000
PART 0
HKLF 4

REM  mo_180609_FI_CeNioda_0m_a.res in P6/mcc
REM R1 =  0.0267 for     890 Fo > 4sig(Fo)  and  0.0272 for all     923 data
REM     83 parameters refined using     83 restraints

END

WGHT      0.0763      2.9486

REM Highest difference peak  0.622,  deepest hole -0.592,  1-sigma level  0.112
Q1    1   0.8641  0.0359  0.3158  11.00000  0.05    0.62
Q2    1   1.0137  0.2414  0.4625  11.00000  0.05    0.57
Q3    1   1.0825  0.1762  0.3702  11.00000  0.05    0.44
Q4    1   0.9759  0.4879  0.2500  10.50000  0.05    0.21
Q5    1   0.7687  0.2754  0.2174  11.00000  0.05    0.19
Q6    1   0.9137  0.3521  0.4497  11.00000  0.05    0.19
Q7    1   0.7847  0.3225  0.5000  10.50000  0.05    0.17
Q8    1   0.8006  0.4953  0.4630  11.00000  0.05    0.17
Q9    1   0.9891  0.3804  0.4714  11.00000  0.05    0.17
Q10   1   0.7173  0.4848  0.5000  10.50000  0.05    0.17
Q11   1   1.0434  0.5229  0.4372  11.00000  0.05    0.17
Q12   1   0.7175  0.3385  0.5000  10.50000  0.05    0.17
Q13   1   0.9233  0.4198  0.4541  11.00000  0.05    0.16
Q14   1   0.8837  0.5578  0.5221  11.00000  0.05    0.14
Q15   1   0.8620  0.2339  0.4660  11.00000  0.05    0.13
Q16   1   0.9406  0.4549  0.3792  11.00000  0.05    0.12
Q17   1   1.1585  0.3915  0.4733  11.00000  0.05    0.12
Q18   1   1.0267  0.4878  0.4389  11.00000  0.05    0.12
Q19   1   0.9234  0.3554  0.2237  11.00000  0.05    0.11
Q20   1   0.8107  0.3906  0.2891  11.00000  0.05    0.11
;
_shelx_res_checksum              5405

_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_preparation       'proton conductor'
####################################################################### 
# 
# 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_mo_180508_FI_LuNioda
_database_code_depnum_ccdc_archive 'CCDC 1987752'
loop_
_audit_author_name
_audit_author_address
'Leopoldo Suescun'
;Facultad de Quimica, Universidad de la Republica, Uruguay
Uruguay
;
_audit_update_record             
;
2020-03-02 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
# start Validation Reply Form

_vrf_PLAT906_mo_180508_FI_LuNioda 
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.032 Check 
RESPONSE: It is a frequent problem of area detectors to overestimate the
background and let some low intensity reflections underestimated. For this
reason, for a small number of low intensity reflections below 1% of Fcmax
a rather large K value is found.
;
_vrf_PLAT976_mo_180508_FI_LuNioda 
;
PROBLEM: Check Calcd Resid. Dens.  1.06A   From O2W            -0.45 eA-3  
RESPONSE: O2W corresponds to a fairly disordered water molecule inside the
compound's voids, this causes the appearance of residual electron density 
surrounding the atom.
;
_vrf_PLAT978_mo_180508_FI_LuNioda 
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: The presence of a heavy atom (Lu and Ni) nucleating most of the 
residual electron density and the low resolution of the data, caused by 
the small crystalline size made it impossible to observe the very small 
electron density residues associated with bonding electrons.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H36 Lu2 Ni3 O38.52'
_chemical_formula_weight         1466.90

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           228
_space_group_name_H-M_alt        'F d -3 c'
_space_group_name_Hall           '-F 4cvw 2vw 3'

_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+1/4, -y+3/4, z+1/2'
'-x+3/4, y+1/2, -z+1/4'
'x+1/2, -y+1/4, -z+3/4'
'z, x, y'
'z+1/2, -x+1/4, -y+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+3/4, x+1/2, -y+1/4'
'y, z, x'
'-y+3/4, z+1/2, -x+1/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'y+3/4, x+1/4, -z'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/4, -x, z+3/4'
'-y, x+3/4, z+1/4'
'x+3/4, z+1/4, -y'
'-x, z+3/4, y+1/4'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/4, -z, y+3/4'
'z+3/4, y+1/4, -x'
'z+1/4, -y, x+3/4'
'-z, y+3/4, x+1/4'
'-z+1/2, -y+1/2, -x+1/2'
'x, y+1/2, z+1/2'
'-x+1/4, -y+5/4, z+1'
'-x+3/4, y+1, -z+3/4'
'x+1/2, -y+3/4, -z+5/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+3/4, -y+5/4'
'-z+1/4, -x+5/4, y+1'
'-z+3/4, x+1, -y+3/4'
'y, z+1/2, x+1/2'
'-y+3/4, z+1, -x+3/4'
'y+1/2, -z+3/4, -x+5/4'
'-y+1/4, -z+5/4, x+1'
'y+3/4, x+3/4, -z+1/2'
'-y+1/2, -x+1, -z+1'
'y+1/4, -x+1/2, z+5/4'
'-y, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1/2'
'-x, z+5/4, y+3/4'
'-x+1/2, -z+1, -y+1'
'x+1/4, -z+1/2, y+5/4'
'z+3/4, y+3/4, -x+1/2'
'z+1/4, -y+1/2, x+5/4'
'-z, y+5/4, x+3/4'
'-z+1/2, -y+1, -x+1'
'x+1/2, y, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+5/4, y+1/2, -z+3/4'
'x+1, -y+1/4, -z+5/4'
'z+1/2, x, y+1/2'
'z+1, -x+1/4, -y+5/4'
'-z+3/4, -x+3/4, y+1'
'-z+5/4, x+1/2, -y+3/4'
'y+1/2, z, x+1/2'
'-y+5/4, z+1/2, -x+3/4'
'y+1, -z+1/4, -x+5/4'
'-y+3/4, -z+3/4, x+1'
'y+5/4, x+1/4, -z+1/2'
'-y+1, -x+1/2, -z+1'
'y+3/4, -x, z+5/4'
'-y+1/2, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+3/4'
'-x+1, -z+1/2, -y+1'
'x+3/4, -z, y+5/4'
'z+5/4, y+1/4, -x+1/2'
'z+3/4, -y, x+5/4'
'-z+1/2, y+3/4, x+3/4'
'-z+1, -y+1/2, -x+1'
'x+1/2, y+1/2, z'
'-x+3/4, -y+5/4, z+1/2'
'-x+5/4, y+1, -z+1/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x+1/2, y'
'z+1, -x+3/4, -y+3/4'
'-z+3/4, -x+5/4, y+1/2'
'-z+5/4, x+1, -y+1/4'
'y+1/2, z+1/2, x'
'-y+5/4, z+1, -x+1/4'
'y+1, -z+3/4, -x+3/4'
'-y+3/4, -z+5/4, x+1/2'
'y+5/4, x+3/4, -z'
'-y+1, -x+1, -z+1/2'
'y+3/4, -x+1/2, z+3/4'
'-y+1/2, x+5/4, z+1/4'
'x+5/4, z+3/4, -y'
'-x+1/2, z+5/4, y+1/4'
'-x+1, -z+1, -y+1/2'
'x+3/4, -z+1/2, y+3/4'
'z+5/4, y+3/4, -x'
'z+3/4, -y+1/2, x+3/4'
'-z+1/2, y+5/4, x+1/4'
'-z+1, -y+1, -x+1/2'
'-x, -y, -z'
'x-1/4, y-3/4, -z-1/2'
'x-3/4, -y-1/2, z-1/4'
'-x-1/2, y-1/4, z-3/4'
'-z, -x, -y'
'-z-1/2, x-1/4, y-3/4'
'z-1/4, x-3/4, -y-1/2'
'z-3/4, -x-1/2, y-1/4'
'-y, -z, -x'
'y-3/4, -z-1/2, x-1/4'
'-y-1/2, z-1/4, x-3/4'
'y-1/4, z-3/4, -x-1/2'
'-y-3/4, -x-1/4, z'
'y-1/2, x-1/2, z-1/2'
'-y-1/4, x, -z-3/4'
'y, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y'
'x, -z-3/4, -y-1/4'
'x-1/2, z-1/2, y-1/2'
'-x-1/4, z, -y-3/4'
'-z-3/4, -y-1/4, x'
'-z-1/4, y, -x-3/4'
'z, -y-3/4, -x-1/4'
'z-1/2, y-1/2, x-1/2'
'-x, -y+1/2, -z+1/2'
'x-1/4, y-1/4, -z'
'x-3/4, -y, z+1/4'
'-x-1/2, y+1/4, z-1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x+1/4, y-1/4'
'z-1/4, x-1/4, -y'
'z-3/4, -x, y+1/4'
'-y, -z+1/2, -x+1/2'
'y-3/4, -z, x+1/4'
'-y-1/2, z+1/4, x-1/4'
'y-1/4, z-1/4, -x'
'-y-3/4, -x+1/4, z+1/2'
'y-1/2, x, z'
'-y-1/4, x+1/2, -z-1/4'
'y, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y+1/2'
'x, -z-1/4, -y+1/4'
'x-1/2, z, y'
'-x-1/4, z+1/2, -y-1/4'
'-z-3/4, -y+1/4, x+1/2'
'-z-1/4, y+1/2, -x-1/4'
'z, -y-1/4, -x+1/4'
'z-1/2, y, x'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-3/4, -z'
'x-1/4, -y-1/2, z+1/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-1/4, y-1/4'
'z+1/4, x-3/4, -y'
'z-1/4, -x-1/2, y+1/4'
'-y+1/2, -z, -x+1/2'
'y-1/4, -z-1/2, x+1/4'
'-y, z-1/4, x-1/4'
'y+1/4, z-3/4, -x'
'-y-1/4, -x-1/4, z+1/2'
'y, x-1/2, z'
'-y+1/4, x, -z-1/4'
'y+1/2, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y+1/2'
'x+1/2, -z-3/4, -y+1/4'
'x, z-1/2, y'
'-x+1/4, z, -y-1/4'
'-z-1/4, -y-1/4, x+1/2'
'-z+1/4, y, -x-1/4'
'z+1/2, -y-3/4, -x+1/4'
'z, y-1/2, x'
'-x+1/2, -y+1/2, -z'
'x+1/4, y-1/4, -z-1/2'
'x-1/4, -y, z-1/4'
'-x, y+1/4, z-3/4'
'-z+1/2, -x+1/2, -y'
'-z, x+1/4, y-3/4'
'z+1/4, x-1/4, -y-1/2'
'z-1/4, -x, y-1/4'
'-y+1/2, -z+1/2, -x'
'y-1/4, -z, x-1/4'
'-y, z+1/4, x-3/4'
'y+1/4, z-1/4, -x-1/2'
'-y-1/4, -x+1/4, z'
'y, x, z-1/2'
'-y+1/4, x+1/2, -z-3/4'
'y+1/2, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y'
'x+1/2, -z-1/4, -y-1/4'
'x, z, y-1/2'
'-x+1/4, z+1/2, -y-3/4'
'-z-1/4, -y+1/4, x'
'-z+1/4, y+1/2, -x-3/4'
'z+1/2, -y-1/4, -x-1/4'
'z, y, x-1/2'

_cell_length_a                   25.296(5)
_cell_length_b                   25.296(5)
_cell_length_c                   25.296(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16186(10)
_cell_formula_units_Z            16
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    15036
_cell_measurement_theta_min      3.794
_cell_measurement_theta_max      24.22

_exptl_crystal_description       cubic
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.408
_exptl_crystal_F_000             11426
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.202
_exptl_absorpt_coefficient_mu    6.332
_shelx_estimated_absorpt_T_min   0.344
_shelx_estimated_absorpt_T_max   0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 10.83333
_diffrn_reflns_number            217123
_diffrn_reflns_av_unetI/netI     0.0067
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.789
_diffrn_reflns_theta_max         29.121
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             922
_reflns_number_gt                715
_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.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²+127.5490P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         922
_refine_ls_number_parameters     66
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0853
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_restrained_S_all      1.287
_refine_ls_shift/su_max          0.000
_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
Lu1 Lu 0.5000 0.2500 0.5000 0.01319(14) Uani 1 6 d S T P . .
C1 C 0.49643(12) 0.37784(15) 0.50830(15) 0.0205(7) Uani 1 1 d . . . . .
C2 C 0.55508(14) 0.37132(14) 0.50230(16) 0.0310(8) Uani 1 1 d D . . . .
H1A H 0.5735(13) 0.3858(14) 0.5324(8) 0.037 Uiso 1 1 d D U . . .
H1B H 0.5681(15) 0.3872(14) 0.4702(7) 0.037 Uiso 1 1 d D U . . .
O1 O 0.46890(9) 0.33602(9) 0.50866(10) 0.0255(5) Uani 1 1 d . . . . .
Ni1 Ni 0.5000 0.5000 0.5000 0.0114(3) Uani 1 6 d S T P . .
O2 O 0.47677(9) 0.42275(9) 0.51321(9) 0.0224(5) Uani 1 1 d . . . . .
Ni2 Ni 0.3750 0.3750 0.3750 0.0273(3) Uani 1 12 d S T P . .
O3 O 0.56707(9) 0.31707(9) 0.5000 0.0228(7) Uani 1 2 d S T P . .
O1W O 0.3750 0.3750 0.45547(15) 0.0409(10) Uani 1 2 d S T P . .
H1W H 0.4011(3) 0.3718(18) 0.4747(7) 0.049 Uiso 1 1 d D U . . .
O2W O 0.3750 0.3750 0.5822(6) 0.076(4) Uani 0.42 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Lu1 0.01319(14) 0.01319(14) 0.01319(14) -0.00244(5) 0.00244(5) -0.00244(5)
C1 0.0233(16) 0.0206(19) 0.0175(13) -0.0022(11) -0.0015(11) 0.0006(11)
C2 0.0225(16) 0.0162(16) 0.054(2) -0.0024(14) 0.0054(15) -0.0009(12)
O1 0.0209(11) 0.0173(11) 0.0383(14) -0.0043(9) 0.0022(10) -0.0016(9)
Ni1 0.0114(3) 0.0114(3) 0.0114(3) -0.00046(15) -0.00046(15) -0.00046(15)
O2 0.0238(11) 0.0182(11) 0.0251(11) 0.0010(9) 0.0015(9) 0.0004(9)
Ni2 0.0273(3) 0.0273(3) 0.0273(3) 0.000 0.000 0.000
O3 0.0165(9) 0.0165(9) 0.0356(19) -0.0035(8) 0.0035(8) 0.0015(11)
O1W 0.0279(19) 0.067(3) 0.0279(19) 0.000 0.000 0.007(2)
O2W 0.070(9) 0.097(11) 0.060(9) 0.000 0.000 -0.017(9)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O1 2.324(2) 18_645 ?
Lu1 O1 2.324(2) 60_554 ?
Lu1 O1 2.324(2) 72 ?
Lu1 O1 2.324(2) 85_446 ?
Lu1 O1 2.324(2) 78_455 ?
Lu1 O1 2.324(2) . ?
Lu1 O3 2.399(3) 78_455 ?
Lu1 O3 2.399(3) 60_554 ?
Lu1 O3 2.399(3) . ?
C1 O2 1.247(4) . ?
C1 O1 1.267(4) . ?
C1 C2 1.500(5) . ?
C2 O3 1.407(4) . ?
C2 H1A 0.964(10) . ?
C2 H1B 0.965(10) . ?
Ni1 O2 2.068(2) . ?
Ni1 O2 2.068(2) 105_666 ?
Ni1 O2 2.068(2) 9 ?
Ni1 O2 2.068(2) 5 ?
Ni1 O2 2.068(2) 101_666 ?
Ni1 O2 2.068(2) 97_666 ?
Ni2 O1W 2.035(4) 50_554 ?
Ni2 O1W 2.035(4) . ?
Ni2 O1W 2.036(4) 83_455 ?
Ni2 O1W 2.036(4) 27_545 ?
Ni2 O1W 2.036(4) 5 ?
Ni2 O1W 2.036(4) 55_554 ?
Ni2 O1W 2.036(4) 9 ?
O3 C2 1.407(4) 85_446 ?
O1W O1W 0.000(8) 50_554 ?
O1W H1W 0.824(10) . ?

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 Lu1 O1 130.00(11) 18_645 60_554 ?
O1 Lu1 O1 78.65(9) 18_645 72 ?
O1 Lu1 O1 86.45(12) 60_554 72 ?
O1 Lu1 O1 78.65(9) 18_645 85_446 ?
O1 Lu1 O1 144.36(12) 60_554 85_446 ?
O1 Lu1 O1 78.65(9) 72 85_446 ?
O1 Lu1 O1 144.36(12) 18_645 78_455 ?
O1 Lu1 O1 78.65(9) 60_554 78_455 ?
O1 Lu1 O1 130.00(11) 72 78_455 ?
O1 Lu1 O1 86.45(12) 85_446 78_455 ?
O1 Lu1 O1 86.45(12) 18_645 . ?
O1 Lu1 O1 78.65(9) 60_554 . ?
O1 Lu1 O1 144.36(12) 72 . ?
O1 Lu1 O1 130.00(12) 85_446 . ?
O1 Lu1 O1 78.65(9) 78_455 . ?
O1 Lu1 O3 136.77(6) 18_645 78_455 ?
O1 Lu1 O3 72.18(6) 60_554 78_455 ?
O1 Lu1 O3 65.00(6) 72 78_455 ?
O1 Lu1 O3 72.18(6) 85_446 78_455 ?
O1 Lu1 O3 65.00(6) 78_455 78_455 ?
O1 Lu1 O3 136.77(6) . 78_455 ?
O1 Lu1 O3 65.00(6) 18_645 60_554 ?
O1 Lu1 O3 65.00(6) 60_554 60_554 ?
O1 Lu1 O3 72.18(6) 72 60_554 ?
O1 Lu1 O3 136.77(6) 85_446 60_554 ?
O1 Lu1 O3 136.77(6) 78_455 60_554 ?
O1 Lu1 O3 72.18(6) . 60_554 ?
O3 Lu1 O3 120.0 78_455 60_554 ?
O1 Lu1 O3 72.18(6) 18_645 . ?
O1 Lu1 O3 136.77(6) 60_554 . ?
O1 Lu1 O3 136.77(6) 72 . ?
O1 Lu1 O3 65.00(6) 85_446 . ?
O1 Lu1 O3 72.18(6) 78_455 . ?
O1 Lu1 O3 65.00(6) . . ?
O3 Lu1 O3 120.0 78_455 . ?
O3 Lu1 O3 120.0 60_554 . ?
O2 C1 O1 122.8(3) . . ?
O2 C1 C2 120.3(3) . . ?
O1 C1 C2 116.9(3) . . ?
O3 C2 C1 108.9(3) . . ?
O3 C2 H1A 107(2) . . ?
C1 C2 H1A 111(2) . . ?
O3 C2 H1B 107(2) . . ?
C1 C2 H1B 112(2) . . ?
H1A C2 H1B 110.0(15) . . ?
C1 O1 Lu1 126.5(2) . . ?
O2 Ni1 O2 94.01(9) . 105_666 ?
O2 Ni1 O2 85.99(9) . 9 ?
O2 Ni1 O2 180.0 105_666 9 ?
O2 Ni1 O2 85.99(9) . 5 ?
O2 Ni1 O2 94.01(9) 105_666 5 ?
O2 Ni1 O2 85.99(9) 9 5 ?
O2 Ni1 O2 94.01(9) . 101_666 ?
O2 Ni1 O2 85.99(9) 105_666 101_666 ?
O2 Ni1 O2 94.01(9) 9 101_666 ?
O2 Ni1 O2 180.00(4) 5 101_666 ?
O2 Ni1 O2 180.0 . 97_666 ?
O2 Ni1 O2 85.99(9) 105_666 97_666 ?
O2 Ni1 O2 94.01(9) 9 97_666 ?
O2 Ni1 O2 94.01(9) 5 97_666 ?
O2 Ni1 O2 85.99(9) 101_666 97_666 ?
C1 O2 Ni1 137.0(2) . . ?
O1W Ni2 O1W 0.0 50_554 . ?
O1W Ni2 O1W 90.0 50_554 83_455 ?
O1W Ni2 O1W 90.0 . 83_455 ?
O1W Ni2 O1W 180.0 50_554 27_545 ?
O1W Ni2 O1W 180.0 . 27_545 ?
O1W Ni2 O1W 90.0 83_455 27_545 ?
O1W Ni2 O1W 90.000(1) 50_554 5 ?
O1W Ni2 O1W 90.000(1) . 5 ?
O1W Ni2 O1W 90.0 83_455 5 ?
O1W Ni2 O1W 90.0 27_545 5 ?
O1W Ni2 O1W 90.0 50_554 55_554 ?
O1W Ni2 O1W 90.0 . 55_554 ?
O1W Ni2 O1W 90.000(1) 83_455 55_554 ?
O1W Ni2 O1W 90.000(1) 27_545 55_554 ?
O1W Ni2 O1W 180.0 5 55_554 ?
O1W Ni2 O1W 90.0 50_554 9 ?
O1W Ni2 O1W 90.0 . 9 ?
O1W Ni2 O1W 180.0 83_455 9 ?
O1W Ni2 O1W 90.0 27_545 9 ?
O1W Ni2 O1W 90.000(1) 5 9 ?
O1W Ni2 O1W 90.0 55_554 9 ?
C2 O3 C2 115.0(4) 85_446 . ?
C2 O3 Lu1 122.51(18) 85_446 . ?
C2 O3 Lu1 122.51(18) . . ?
O1W O1W Ni2 0(10) 50_554 . ?
O1W O1W H1W 0(10) 50_554 . ?
Ni2 O1W H1W 126.1(11) . . ?

_refine_diff_density_max         0.373
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.185

_shelx_res_file                  
;

    mo_180508_FI_LuNioda.res created by SHELXL-2014/7


TITL mo_180508_FI_LuNioda_0m_n.res in Fd-3c
REM Old TITL mo_180508_FI_LuNioda_0m in Fd-3c

REM SHELXT solution in Fd-3c
REM R1 0.910,  Rweak 0.001,  Alpha 0.097,  Orientation as input
REM Formula found by SHELXT:  C66 O3 Ni2 Lu2

CELL  0.71073  25.2958  25.2958  25.2958   90.000   90.000   90.000
ZERR    16.000   0.0050   0.0050   0.0050    0.000    0.000    0.000
LATT  4
SYMM 1/4-X, 3/4-Y, 1/2+Z
SYMM 3/4-X, 1/2+Y, 1/4-Z
SYMM 1/2+X, 1/4-Y, 3/4-Z
SYMM Z, X, Y
SYMM 1/2+Z, 1/4-X, 3/4-Y
SYMM 1/4-Z, 3/4-X, 1/2+Y
SYMM 3/4-Z, 1/2+X, 1/4-Y
SYMM Y, Z, X
SYMM 3/4-Y, 1/2+Z, 1/4-X
SYMM 1/2+Y, 1/4-Z, 3/4-X
SYMM 1/4-Y, 3/4-Z, 1/2+X
SYMM 3/4+Y, 1/4+X, -Z
SYMM 1/2-Y, 1/2-X, 1/2-Z
SYMM 1/4+Y, -X, 3/4+Z
SYMM -Y, 3/4+X, 1/4+Z
SYMM 3/4+X, 1/4+Z, -Y
SYMM -X, 3/4+Z, 1/4+Y
SYMM 1/2-X, 1/2-Z, 1/2-Y
SYMM 1/4+X, -Z, 3/4+Y
SYMM 3/4+Z, 1/4+Y, -X
SYMM 1/4+Z, -Y, 3/4+X
SYMM -Z, 3/4+Y, 1/4+X
SYMM 1/2-Z, 1/2-Y, 1/2-X
SFAC C H O NI LU
UNIT 384 576 616.3 48 32
EQIV $1 3/4-X, +Y, 3/4-Z
EQIV $2 3/4-x, 3/4-y, +z
TEMP 25
L.S. 10
ACTA
SIZE 0.202 0.206 0.214
BOND $H
LIST 6
FMAP 2
PLAN 20
WGHT    0.032800  127.549011
FVAR       0.02311
LU1   5    0.500000    0.250000    0.500000    10.16667    0.01319    0.01319 =
         0.01319   -0.00244    0.00244   -0.00244
C1    1    0.496433    0.377836    0.508295    11.00000    0.02334    0.02061 =
         0.01749   -0.00215   -0.00151    0.00055
DFIX 0.97 0.01 C2 H1A
DFIX 0.97 0.01 C2 H1B
DANG 1.575 0.01 H1A H1B
C2    1    0.555077    0.371321    0.502298    11.00000    0.02249    0.01623 =
         0.05419   -0.00235    0.00539   -0.00086
H1A   2    0.573462    0.385814    0.532385    11.00000   -1.20000
H1B   2    0.568106    0.387211    0.470162    11.00000   -1.20000
O1    3    0.468896    0.336015    0.508659    11.00000    0.02091    0.01734 =
         0.03831   -0.00430    0.00220   -0.00160
NI1   4    0.500000    0.500000    0.500000    10.16667    0.01139    0.01139 =
         0.01139   -0.00046   -0.00046   -0.00046
O2    3    0.476766    0.422750    0.513207    11.00000    0.02381    0.01822 =
         0.02512    0.00104    0.00150    0.00036
NI2   4    0.375000    0.375000    0.375000    10.08333    0.02734    0.02734 =
         0.02734    0.00000    0.00000    0.00000
O3    3    0.567067    0.317067    0.500000    10.50000    0.01648    0.01648 =
         0.03558   -0.00346    0.00346    0.00148
DFIX 0.83 0.01 O1W_$2 H1W
DANG 1.33 0.01 H1W H1W_$2
O1W   3    0.375000    0.375000    0.455468    10.50000    0.02790    0.06685 =
         0.02788    0.00000    0.00000    0.00738
H1W   2    0.401117    0.371750    0.474669    11.00000   -1.20000
O2W   3    0.375000    0.375000    0.582236    10.21000    0.06977    0.09669 =
         0.06040    0.00000    0.00000   -0.01697
HKLF 4

REM  mo_180508_FI_LuNioda_0m_n.res in Fd-3c
REM R1 =  0.0279 for     715 Fo > 4sig(Fo)  and  0.0377 for all     922 data
REM     66 parameters refined using      5 restraints

END

WGHT      0.0328    127.5764

REM Highest difference peak  0.373,  deepest hole -1.219,  1-sigma level  0.185
Q1    1   0.4248  0.4181  0.5201  11.00000  0.05    0.37
Q2    1   0.3356  0.3902  0.5884  11.00000  0.05    0.36
Q3    1   0.4228  0.3313  0.5531  11.00000  0.05    0.35
Q4    1   0.3501  0.3297  0.4216  11.00000  0.05    0.35
Q5    1   0.5000  0.3185  0.5685  10.50000  0.05    0.35
Q6    1   0.4422  0.4216  0.5437  11.00000  0.05    0.34
Q7    1   0.5664  0.3892  0.5517  11.00000  0.05    0.33
Q8    1   0.4498  0.4297  0.5513  11.00000  0.05    0.33
Q9    1   0.4349  0.4182  0.5277  11.00000  0.05    0.33
Q10   1   0.3381  0.4015  0.5699  11.00000  0.05    0.33
Q11   1   0.4288  0.3212  0.4288  10.33333  0.05    0.32
Q12   1   0.3387  0.3642  0.5723  11.00000  0.05    0.32
Q13   1   0.3833  0.4082  0.5916  11.00000  0.05    0.32
Q14   1   0.4485  0.3159  0.5580  11.00000  0.05    0.32
Q15   1   0.5766  0.4379  0.4535  11.00000  0.05    0.32
Q16   1   0.5907  0.4020  0.5755  11.00000  0.05    0.31
Q17   1   0.4115  0.4071  0.5281  11.00000  0.05    0.31
Q18   1   0.5776  0.3491  0.5713  11.00000  0.05    0.31
Q19   1   0.5812  0.3976  0.5046  11.00000  0.05    0.31
Q20   1   0.3511  0.4128  0.5609  11.00000  0.05    0.31
;
_shelx_res_checksum              24256

_exptl_crystal_recrystallization_method hydrothermal
