# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_Nd_sq
_database_code_depnum_ccdc_archive 'CCDC 2215184'
loop_
_audit_author_name
_audit_author_address
'Zhanning Liu'
;Shandong University of Science and Technology 
China
;
_audit_update_record             
;
2022-10-25 deposited with the CCDC.	2022-11-21 downloaded from the CCDC.
;
_audit_creation_date             2022-10-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C16 Nd2 O16)'
_chemical_formula_sum            'C8 Nd O8'
_chemical_formula_weight         368.32
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           125
_space_group_name_H-M_alt        'P 4/n b m'
_space_group_name_Hall           '-P 4a 2b'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'x, -y+1/2, -z'
'-x+1/2, y, -z'
'y, x, -z'
'-y+1/2, -x+1/2, -z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
'-x, y-1/2, z'
'x-1/2, -y, z'
'-y, -x, z'
'y-1/2, x-1/2, z'

_cell_length_a                   10.0014(2)
_cell_length_b                   10.0014(2)
_cell_length_c                   5.4087(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     541.02(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1347
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.4190
_cell_measurement_theta_min      6.2400
_shelx_estimated_absorpt_T_max   0.404
_shelx_estimated_absorpt_T_min   0.119
_exptl_absorpt_coefficient_mu    36.949
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.743
_diffrn_reflns_Laue_measured_fraction_max 0.745
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            1831
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.745
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.567
_diffrn_reflns_theta_min         12.120
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.743
_diffrn_measured_fraction_theta_max 0.745
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                193
_reflns_number_total             216
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.046
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     21
_refine_ls_number_reflns         216
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0267
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0586P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0697
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(Nd1) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_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 0.250000 0.250000 0.500000 0.00025(17) Uani 1 8 d S TU P . .
O2 O 0.3327(2) 0.0591(2) 0.2631(5) 0.0189(5) Uani 1 1 d . . . . .
C4 C 0.4241(4) 0.0272(4) 0.1208(7) 0.0095(6) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nd1 0.00019(16) 0.00019(16) 0.0004(2) 0.000 0.000 0.000
O2 0.0160(12) 0.0146(12) 0.0260(12) -0.0054(9) 0.0140(10) 0.0019(9)
C4 0.0069(16) 0.0071(17) 0.0143(19) 0.0017(16) -0.0012(14) 0.0003(14)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O2 2.443(2) . ?
Nd1 O2 2.443(2) 6_556 ?
Nd1 O2 2.443(2) 7_556 ?
Nd1 O2 2.443(2) 5_556 ?
Nd1 O2 2.443(2) 3 ?
Nd1 O2 2.443(2) 4 ?
Nd1 O2 2.443(2) 8_556 ?
Nd1 O2 2.443(2) 2 ?
O2 C4 1.237(5) . ?
C4 C4 1.477(8) 8 ?
C4 C4 1.459(7) 16_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
O2 Nd1 O2 140.43(12) . 5_556 ?
O2 Nd1 O2 74.03(6) 4 3 ?
O2 Nd1 O2 74.03(6) 6_556 7_556 ?
O2 Nd1 O2 74.03(6) . 4 ?
O2 Nd1 O2 143.51(12) . 7_556 ?
O2 Nd1 O2 143.51(12) 5_556 4 ?
O2 Nd1 O2 143.51(12) 6_556 2 ?
O2 Nd1 O2 75.30(12) . 8_556 ?
O2 Nd1 O2 140.43(12) 6_556 3 ?
O2 Nd1 O2 74.03(6) 5_556 8_556 ?
O2 Nd1 O2 77.25(12) 4 7_556 ?
O2 Nd1 O2 140.44(12) 4 8_556 ?
O2 Nd1 O2 75.30(12) 3 7_556 ?
O2 Nd1 O2 77.25(12) . 6_556 ?
O2 Nd1 O2 77.25(12) 5_556 3 ?
O2 Nd1 O2 116.73(12) 5_556 6_556 ?
O2 Nd1 O2 143.51(12) 8_556 3 ?
O2 Nd1 O2 75.30(12) 4 6_556 ?
O2 Nd1 O2 74.03(6) 2 3 ?
O2 Nd1 O2 74.03(6) 8_556 6_556 ?
O2 Nd1 O2 74.03(6) 5_556 7_556 ?
O2 Nd1 O2 74.03(6) . 2 ?
O2 Nd1 O2 116.73(12) 8_556 7_556 ?
O2 Nd1 O2 75.30(12) 5_556 2 ?
O2 Nd1 O2 140.43(12) 2 7_556 ?
O2 Nd1 O2 116.73(12) 4 2 ?
O2 Nd1 O2 77.25(12) 8_556 2 ?
O2 Nd1 O2 116.73(12) . 3 ?
C4 O2 Nd1 141.1(3) . . ?
O2 C4 C4 135.2(2) . 8 ?
O2 C4 C4 134.8(2) . 16_655 ?
C4 C4 C4 90.0 16_655 8 ?

_shelx_res_file                  
;
TITL Nd_sq in P4/nbm #125
    nd_sq_sq_sqd.res
    created by SHELXL-2016/6 at 13:49:06 on 25-Oct-2022
REM reset to P4/nbm #125
CELL 1.54184 10.001395 10.001395 5.408714 90 90 90
ZERR 8 0.000198 0.000198 0.000211 0 0 0
LATT 1
SYMM 0.5-Y,+X,+Z
SYMM 0.5-X,0.5-Y,+Z
SYMM +Y,0.5-X,+Z
SYMM +X,0.5-Y,-Z
SYMM 0.5-X,+Y,-Z
SYMM +Y,+X,-Z
SYMM 0.5-Y,0.5-X,-Z
SFAC C Nd O
UNIT 16 2 16
ISOR 0.00001 0.00002 Nd1

L.S. 5 0 4
PLAN  20
fmap 2
acta NOHKL
OMIT 0 2 0
OMIT 1 1 0
OMIT 1 3 0
OMIT 3 4 2
OMIT 0 0 1
OMIT 2 3 2
OMIT 4 5 1
OMIT 3 3 6
OMIT 2 4 6
OMIT 6 6 0
OMIT 5 6 2
OMIT 2 2 0
OMIT 1 1 1
OMIT 3 4 3
OMIT 0 2 6
OMIT 1 1 6
OMIT 1 5 6
OMIT 1 2 2
OMIT 2 5 2
OMIT 1 3 6
OMIT 0 4 6
OMIT 6 10 0
OMIT 2 2 6
OMIT 0 0 6
OMIT 3 3 0
OMIT 2 3 3
OMIT 4 4 0
OMIT 1 7 5
OMIT 2 2 5
OMIT 3 6 1
OMIT 6 8 0
OMIT 5 6 1
OMIT 0 2 5
OMIT 3 6 2
OMIT 2 5 1
OMIT 1 3 5
OMIT 4 5 3
OMIT 8 8 0
OMIT 2 2 4
OMIT 2 10 0
OMIT 2 3 1
OMIT 1 4 4
OMIT 0 4 0
OMIT 4 5 2
OMIT 1 4 3
OMIT 4 9 3
OMIT 0 8 5
OMIT 4 6 0
OMIT 0 4 5
OMIT 4 6 5
OMIT 3 7 5
OMIT 4 4 5
OMIT 2 11 1
OMIT 3 5 5
OMIT 4 10 0
OMIT 5 5 5
OMIT 2 6 5
OMIT 3 3 5
OMIT 2 4 0
OMIT 2 4 5
OMIT 0 4 4
OMIT 4 8 0
OMIT 1 5 3
OMIT 1 9 0
OMIT 1 2 3
OMIT 2 2 1
OMIT 3 4 1
OMIT 1 1 5
OMIT 0 10 0
OMIT 3 10 2
OMIT 2 8 0
OMIT 6 8 1
OMIT 1 5 5
REM <olex2.extras>
REM <HklSrc "%.\\Nd_sq.hkl">
REM </olex2.extras>

WGHT    0.058600
FVAR       6.81237
ND1   2    0.250000    0.250000    0.500000    10.12500    0.00019    0.00019 =
         0.00037    0.00000    0.00000    0.00000
O2    3    0.332690    0.059134    0.263053    11.00000    0.01601    0.01456 =
         0.02600   -0.00540    0.01401    0.00190
C4    1    0.424110    0.027241    0.120828    11.00000    0.00694    0.00710 =
         0.01433    0.00171   -0.00122    0.00029
HKLF 4




REM  Nd_sq in P4/nbm #125
REM R1 =  0.0267 for     193 Fo > 4sig(Fo)  and  0.0284 for all     216 data
REM     21 parameters refined using      6 restraints

END

WGHT      0.0586      0.0000

REM Highest difference peak  2.046,  deepest hole -1.406,  1-sigma level  0.151
Q1    1   0.2500  0.2500  0.3871  10.25000  0.05    2.05
Q2    1   0.2500 -0.2500  0.2097  10.25000  0.05    0.77
Q3    1   0.3009 -0.1991  0.5441  10.50000  0.05    0.54
Q4    1   0.2487  0.1628  0.2318  11.00000  0.05    0.52
Q5    1   0.4399  0.0348  0.0028  11.00000  0.05    0.46
Q6    1   0.2500 -0.0726  0.0000  10.50000  0.05    0.32
Q7    1   0.6064  0.1064  0.2162  10.50000  0.05    0.30
Q8    1   0.2799  0.0968  0.3981  11.00000  0.05    0.29
Q9    1   0.1769  0.0506  0.2992  11.00000  0.05    0.26
Q10   1   0.2500  0.0453  0.5000  10.50000  0.05    0.25
Q11   1   0.2441 -0.0941  0.1927  11.00000  0.05    0.25
Q12   1   0.2155 -0.0880  0.4037  11.00000  0.05    0.24
Q13   1   0.5023  0.0396  0.2188  11.00000  0.05    0.24
Q14   1   0.3932 -0.1068  0.0374  10.50000  0.05    0.23
Q15   1   0.3719 -0.0820  0.0116  11.00000  0.05    0.23
Q16   1   0.3443 -0.0529 -0.1003  11.00000  0.05    0.23
Q17   1   0.2500  0.1426  0.5000  10.50000  0.05    0.22
Q18   1   0.5225  0.0224  0.1811  10.50000  0.05    0.22
Q19   1   0.2676  0.0628  0.4044  11.00000  0.05    0.19
Q20   1   0.2490  0.2083  0.1336  11.00000  0.05    0.18
;
_shelx_res_checksum              12368
_olex2_submission_special_instructions 'No special instructions were received'
