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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_20_mf001
_database_code_depnum_ccdc_archive 'CCDC 2078968'
loop_
_audit_author_name
_audit_author_address
'Paul Saines'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2021-04-20 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_audit_creation_date             2021-03-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Holmium Formate Oxalate'
_chemical_formula_moiety         'C3 H Ho O6'
_chemical_formula_sum            'C3 H Ho O6'
_chemical_formula_weight         297.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ho C3 O6 H'
_chemical_oxdiff_usercomment     '150 K'
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'
Ho Ho -14.9734 3.7046 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   6.9473(3)
_cell_length_b                   10.5261(4)
_cell_length_c                   6.5526(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     479.18(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1093
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      71.1660
_cell_measurement_theta_min      7.9730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    30.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    4.130
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2037
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.288
_diffrn_reflns_theta_min         7.966
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -14.00   1.00    2.00    --  -41.66 -57.00 120.00  100
  2  ω    -30.00  70.00   1.00    2.00    --   41.66 -57.00 -90.00  100
  3  ω     94.00 177.00   1.00    8.00    --  103.72 125.00-120.00   83
  4  ω     21.00 109.00   1.00    8.00    --  103.72 -94.00  30.00   88
  5  ω     78.00 177.00   1.00    8.00    --  103.72  45.00 -30.00   99
  6  ω     27.00 132.00   1.00    8.00    --  103.72 -30.00 120.00  105
  7  ω   -114.00 -14.00   1.00    2.00    --  -41.66 -57.00   0.00  100
  8  ω   -114.00 -14.00   1.00    2.00    --  -41.66 -57.00-120.00  100
  9  ω      1.00  47.00   1.00    2.00    --   41.66 -99.00 120.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2093399000
_diffrn_orient_matrix_UB_12      -0.0473099000
_diffrn_orient_matrix_UB_13      -0.0164460000
_diffrn_orient_matrix_UB_21      0.0031649000
_diffrn_orient_matrix_UB_22      0.0361299000
_diffrn_orient_matrix_UB_23      -0.2277350000
_diffrn_orient_matrix_UB_31      0.0730459000
_diffrn_orient_matrix_UB_32      0.1337735000
_diffrn_orient_matrix_UB_33      0.0556654000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                465
_reflns_number_total             489
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         489
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0189
_refine_ls_restrained_S_all      1.042
_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)+(0.0273P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0455
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.20113(4) 0.250000 0.36659(5) 0.00697(14) Uani 1 2 d S T P . .
O4 O 0.0886(3) 0.6239(2) 0.6485(3) 0.0096(5) Uani 1 1 d . . . . .
O3 O 0.2411(3) 0.4540(2) 0.5210(4) 0.0130(5) Uani 1 1 d . . . . .
O2 O 0.5535(4) 0.250000 0.8020(5) 0.0160(7) Uani 1 2 d S T P . .
O1 O 0.5332(4) 0.250000 0.4624(5) 0.0092(6) Uani 1 2 d S T P . .
C2 C 0.0970(4) 0.5217(3) 0.5484(5) 0.0103(6) Uani 1 1 d . . . . .
C1 C 0.6243(6) 0.250000 0.6303(7) 0.0132(10) Uani 1 2 d S T P . .
H1 H 0.760839 0.250000 0.622315 0.016 Uiso 1 2 calc 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
Ho1 0.00647(18) 0.0067(2) 0.0077(2) 0.000 0.00019(11) 0.000
O4 0.0108(9) 0.0063(10) 0.0116(12) -0.0030(8) -0.0015(8) 0.0009(8)
O3 0.0113(9) 0.0099(10) 0.0180(13) -0.0040(9) -0.0013(9) 0.0006(9)
O2 0.0129(15) 0.0240(18) 0.0112(17) 0.000 -0.0019(13) 0.000
O1 0.0088(13) 0.0103(15) 0.0085(15) 0.000 0.0001(12) 0.000
C2 0.0109(14) 0.0091(16) 0.0110(16) -0.0001(12) -0.0002(13) -0.0001(11)
C1 0.011(2) 0.019(2) 0.010(3) 0.000 -0.0025(16) 0.000

_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 Ho1 3.7948(3) 6_556 ?
Ho1 Ho1 3.7948(3) 6_656 ?
Ho1 O4 2.437(2) 2_564 ?
Ho1 O4 2.413(2) 5_566 ?
Ho1 O4 2.437(2) 8_655 ?
Ho1 O4 2.413(2) 3_546 ?
Ho1 O3 2.390(2) . ?
Ho1 O3 2.390(2) 7_565 ?
Ho1 O2 2.402(3) 6_557 ?
Ho1 O1 2.391(3) . ?
Ho1 O1 2.451(3) 6_556 ?
O4 C2 1.261(4) . ?
O3 C2 1.242(4) . ?
O2 C1 1.228(6) . ?
O1 C1 1.269(6) . ?
C2 C2 1.558(6) 5_566 ?
C1 H1 0.9500 . ?

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
Ho1 Ho1 Ho1 132.514(17) 6_656 6_556 ?
O4 Ho1 Ho1 108.22(5) 2_564 6_556 ?
O4 Ho1 Ho1 38.29(5) 2_564 6_656 ?
O4 Ho1 Ho1 38.73(5) 5_566 6_556 ?
O4 Ho1 Ho1 108.22(5) 8_655 6_556 ?
O4 Ho1 Ho1 38.73(5) 3_546 6_556 ?
O4 Ho1 Ho1 138.34(5) 5_566 6_656 ?
O4 Ho1 Ho1 38.29(5) 8_655 6_656 ?
O4 Ho1 Ho1 138.34(5) 3_546 6_656 ?
O4 Ho1 O4 100.17(7) 3_546 8_655 ?
O4 Ho1 O4 140.86(4) 3_546 2_564 ?
O4 Ho1 O4 66.73(10) 3_546 5_566 ?
O4 Ho1 O4 66.00(10) 8_655 2_564 ?
O4 Ho1 O4 140.86(4) 5_566 8_655 ?
O4 Ho1 O4 100.17(7) 5_566 2_564 ?
O4 Ho1 O1 64.34(7) 5_566 6_556 ?
O4 Ho1 O1 64.34(7) 3_546 6_556 ?
O4 Ho1 O1 76.68(7) 2_564 6_556 ?
O4 Ho1 O1 76.68(7) 8_655 6_556 ?
O3 Ho1 Ho1 93.67(6) 7_565 6_656 ?
O3 Ho1 Ho1 106.07(5) 7_565 6_556 ?
O3 Ho1 Ho1 93.67(6) . 6_656 ?
O3 Ho1 Ho1 106.07(5) . 6_556 ?
O3 Ho1 O4 67.68(7) 7_565 3_546 ?
O3 Ho1 O4 131.91(7) . 8_655 ?
O3 Ho1 O4 127.48(8) 7_565 5_566 ?
O3 Ho1 O4 127.48(8) . 3_546 ?
O3 Ho1 O4 71.90(8) . 2_564 ?
O3 Ho1 O4 131.91(7) 7_565 2_564 ?
O3 Ho1 O4 67.68(7) . 5_566 ?
O3 Ho1 O4 71.90(8) 7_565 8_655 ?
O3 Ho1 O3 127.92(12) 7_565 . ?
O3 Ho1 O2 70.54(6) . 6_557 ?
O3 Ho1 O2 70.54(6) 7_565 6_557 ?
O3 Ho1 O1 115.32(6) . 6_556 ?
O3 Ho1 O1 115.32(6) 7_565 6_556 ?
O3 Ho1 O1 77.10(6) 7_565 . ?
O3 Ho1 O1 77.10(6) . . ?
O2 Ho1 Ho1 88.46(7) 6_557 6_556 ?
O2 Ho1 Ho1 139.03(7) 6_557 6_656 ?
O2 Ho1 O4 141.85(6) 6_557 2_564 ?
O2 Ho1 O4 71.38(8) 6_557 5_566 ?
O2 Ho1 O4 141.85(6) 6_557 8_655 ?
O2 Ho1 O4 71.38(8) 6_557 3_546 ?
O2 Ho1 O1 126.29(10) 6_557 6_556 ?
O1 Ho1 Ho1 37.84(7) 6_556 6_556 ?
O1 Ho1 Ho1 171.47(8) . 6_556 ?
O1 Ho1 Ho1 38.96(8) . 6_656 ?
O1 Ho1 Ho1 94.68(7) 6_556 6_656 ?
O1 Ho1 O4 64.88(8) . 2_564 ?
O1 Ho1 O4 64.88(8) . 8_655 ?
O1 Ho1 O4 144.66(6) . 3_546 ?
O1 Ho1 O4 144.66(6) . 5_566 ?
O1 Ho1 O2 100.07(11) . 6_557 ?
O1 Ho1 O1 133.64(9) . 6_556 ?
Ho1 O4 Ho1 102.98(8) 5_566 2_565 ?
C2 O4 Ho1 137.89(19) . 2_565 ?
C2 O4 Ho1 119.09(18) . 5_566 ?
C2 O3 Ho1 118.89(19) . . ?
C1 O2 Ho1 131.1(3) . 6_657 ?
Ho1 O1 Ho1 103.20(12) . 6_656 ?
C1 O1 Ho1 121.7(3) . 6_656 ?
C1 O1 Ho1 135.1(3) . . ?
O4 C2 C2 115.0(3) . 5_566 ?
O3 C2 O4 127.0(3) . . ?
O3 C2 C2 118.0(3) . 5_566 ?
O2 C1 O1 126.5(4) . . ?
O2 C1 H1 116.8 . . ?
O1 C1 H1 116.8 . . ?

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 O4 C2 O3 171.1(3) 5_566 . . . ?
Ho1 O4 C2 O3 -6.2(5) 2_565 . . . ?
Ho1 O4 C2 C2 173.5(2) 2_565 . . 5_566 ?
Ho1 O4 C2 C2 -9.2(4) 5_566 . . 5_566 ?
Ho1 O3 C2 O4 170.9(3) . . . . ?
Ho1 O3 C2 C2 -8.9(5) . . . 5_566 ?
Ho1 O2 C1 O1 180.000(1) 6_657 . . . ?
Ho1 O1 C1 O2 0.000(1) . . . . ?
Ho1 O1 C1 O2 180.000(1) 6_656 . . . ?

_shelx_res_file                  
;
TITL 20_mf001_a.res in Pnma
    20_mf001.res
    created by SHELXL-2018/3 at 21:03:11 on 31-Mar-2021
REM Old TITL 20_MF001 in Pnma #62
REM SHELXT solution in Pnma
REM R1 0.025, Rweak 0.099, Alpha 0.024, Orientation as input
REM Formula found by SHELXT: C3 O6 Ho
CELL 1.54184 6.947274 10.526062 6.552607 90 90 90
ZERR 4 0.000251 0.00043 0.000365 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Ho O
UNIT 12 4 4 24

L.S. 50
PLAN  5
TEMP -153.15
CONF
BOND $H
LIST 6
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\20_MF001.hkl">
REM </olex2.extras>

WGHT    0.027300
FVAR       0.46330
HO1   3    0.201127    0.250000    0.366587    10.50000    0.00647    0.00671 =
         0.00772    0.00000    0.00019    0.00000
O4    4    0.088613    0.623932    0.648498    11.00000    0.01081    0.00629 =
         0.01163   -0.00302   -0.00152    0.00087
O3    4    0.241118    0.454012    0.520987    11.00000    0.01133    0.00986 =
         0.01795   -0.00399   -0.00132    0.00059
O2    4    0.553475    0.250000    0.802003    10.50000    0.01289    0.02402 =
         0.01123    0.00000   -0.00193    0.00000
O1    4    0.533219    0.250000    0.462358    10.50000    0.00879    0.01029 =
         0.00846    0.00000    0.00010    0.00000
C2    1    0.096989    0.521732    0.548396    11.00000    0.01092    0.00909 =
         0.01100   -0.00010   -0.00025   -0.00008
C1    1    0.624301    0.250000    0.630266    10.50000    0.01147    0.01862 =
         0.00960    0.00000   -0.00254    0.00000
AFIX  43
H1    2    0.760839    0.250000    0.622315    10.50000   -1.20000
AFIX   0
HKLF 4




REM  20_mf001_a.res in Pnma
REM wR2 = 0.0455, GooF = S = 1.042, Restrained GooF = 1.042 for all data
REM R1 = 0.0189 for 465 Fo > 4sig(Fo) and 0.0203 for all 489 data
REM 52 parameters refined using 0 restraints

END

WGHT      0.0273      0.0000

REM Highest difference peak  0.592,  deepest hole -0.804,  1-sigma level  0.127
Q1    1   0.2043  0.2500  0.5224  10.50000  0.05    0.59
Q2    1   0.0000  0.5000  0.5000  10.50000  0.05    0.55
Q3    1   0.2000  0.2500  0.2074  10.50000  0.05    0.51
Q4    1   0.2135  0.6218  0.8137  11.00000  0.05    0.44
Q5    1  -0.0607  0.6390  0.6366  11.00000  0.05    0.44
;
_shelx_res_checksum              35308
_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 1.649
_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_20_mf002
_database_code_depnum_ccdc_archive 'CCDC 2078969'
loop_
_audit_author_name
_audit_author_address
'Paul Saines'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2021-04-20 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_audit_creation_date             2021-04-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Erbium formate oxalate'
_chemical_formula_moiety         'C3 H Er O6'
_chemical_formula_sum            'C3 H Er O6'
_chemical_formula_weight         300.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Er C3 O6 H'
_chemical_oxdiff_usercomment     '150 K'
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'
Er Er -9.4367 3.9380 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   6.9198(4)
_cell_length_b                   10.4921(6)
_cell_length_c                   6.5331(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     474.32(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    617
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      70.7360
_cell_measurement_theta_min      7.9860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    32.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    4.205
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             540
_exptl_crystal_preparation       'solvothermal synthesis'
_exptl_crystal_size_max          0.063
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.015
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1003
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.804
_diffrn_reflns_theta_min         7.990
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00  -4.00   1.00    3.62    --  -42.16 125.00 120.00   48
  2  ω    -60.00  28.00   1.00    3.62    --  -42.16  57.00  90.00   88
  3  ω    119.00 159.00   1.00   14.46    --  103.72 125.00-180.00   40
  4  ω     45.00 101.00   1.00   14.46    --  103.72 -94.00 150.00   56
  5  ω     28.00 125.00   1.00   14.46    --  103.72 -77.00-120.00   97
  6  ω     21.00  69.00   1.00   14.46    --  103.72 -94.00 120.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1226448000
_diffrn_orient_matrix_UB_12      0.0582461000
_diffrn_orient_matrix_UB_13      -0.1732011000
_diffrn_orient_matrix_UB_21      0.1206426000
_diffrn_orient_matrix_UB_22      -0.1233382000
_diffrn_orient_matrix_UB_23      -0.0110476000
_diffrn_orient_matrix_UB_31      -0.1414300000
_diffrn_orient_matrix_UB_32      -0.0544870000
_diffrn_orient_matrix_UB_33      -0.1594066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                447
_reflns_number_total             483
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0190
_refine_ls_restrained_S_all      1.041
_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)+(0.0245P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0430
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.79954(4) 0.750000 0.63360(4) 0.00421(13) Uani 1 2 d S T P . .
O4 O 0.9104(4) 0.3760(3) 0.3505(4) 0.0072(5) Uani 1 1 d . . . . .
O2 O 0.4470(6) 0.750000 0.1965(7) 0.0148(10) Uani 1 2 d S T P . .
O1 O 0.4678(6) 0.750000 0.5383(6) 0.0070(8) Uani 1 2 d S T P . .
O3 O 0.7582(4) 0.5464(3) 0.4790(5) 0.0100(6) Uani 1 1 d . . . . .
C1 C 0.3762(8) 0.750000 0.3683(9) 0.0104(12) Uani 1 2 d S T P . .
H1 H 0.239102 0.750000 0.376081 0.012 Uiso 1 2 calc R U P . .
C2 C 0.9032(6) 0.4791(4) 0.4519(6) 0.0079(8) 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
Er1 0.00467(17) 0.00530(18) 0.00266(19) 0.000 0.00022(12) 0.000
O4 0.0073(11) 0.0081(13) 0.0062(12) -0.0010(11) -0.0013(11) 0.0015(11)
O2 0.014(2) 0.023(3) 0.008(2) 0.000 -0.0025(16) 0.000
O1 0.0078(17) 0.009(2) 0.0040(17) 0.000 -0.0010(15) 0.000
O3 0.0082(11) 0.0059(12) 0.0160(14) -0.0026(11) 0.0012(11) -0.0002(11)
C1 0.007(2) 0.020(3) 0.004(3) 0.000 0.001(2) 0.000
C2 0.0103(19) 0.010(2) 0.0034(17) -0.0009(14) -0.0001(15) 0.0007(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
Er1 Er1 3.7794(3) 6_657 ?
Er1 Er1 3.7794(3) 6_557 ?
Er1 O4 2.422(3) 2_665 ?
Er1 O4 2.406(3) 3_756 ?
Er1 O4 2.406(3) 5_766 ?
Er1 O4 2.422(3) 8_766 ?
Er1 O2 2.386(4) 6_656 ?
Er1 O1 2.379(4) . ?
Er1 O1 2.439(4) 6_657 ?
Er1 O3 2.380(3) 7_575 ?
Er1 O3 2.380(3) . ?
O4 C2 1.269(5) . ?
O2 C1 1.225(8) . ?
O1 C1 1.279(7) . ?
O3 C2 1.239(5) . ?
C1 H1 0.9500 . ?
C2 C2 1.543(8) 5_766 ?

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
Er1 Er1 Er1 132.542(16) 6_657 6_557 ?
O4 Er1 Er1 138.27(7) 3_756 6_557 ?
O4 Er1 Er1 108.29(6) 8_766 6_657 ?
O4 Er1 Er1 38.32(7) 8_766 6_557 ?
O4 Er1 Er1 108.29(6) 2_665 6_657 ?
O4 Er1 Er1 38.64(7) 5_766 6_657 ?
O4 Er1 Er1 138.27(7) 5_766 6_557 ?
O4 Er1 Er1 38.32(7) 2_665 6_557 ?
O4 Er1 Er1 38.64(7) 3_756 6_657 ?
O4 Er1 O4 100.08(10) 3_756 8_766 ?
O4 Er1 O4 140.82(5) 5_766 8_766 ?
O4 Er1 O4 140.82(5) 3_756 2_665 ?
O4 Er1 O4 100.08(10) 5_766 2_665 ?
O4 Er1 O4 66.17(14) 8_766 2_665 ?
O4 Er1 O4 66.69(14) 3_756 5_766 ?
O4 Er1 O1 64.14(10) 5_766 6_657 ?
O4 Er1 O1 64.14(10) 3_756 6_657 ?
O4 Er1 O1 76.84(10) 2_665 6_657 ?
O4 Er1 O1 76.84(10) 8_766 6_657 ?
O2 Er1 Er1 139.05(10) 6_656 6_557 ?
O2 Er1 Er1 88.41(10) 6_656 6_657 ?
O2 Er1 O4 141.75(8) 6_656 8_766 ?
O2 Er1 O4 71.48(11) 6_656 5_766 ?
O2 Er1 O4 71.48(11) 6_656 3_756 ?
O2 Er1 O4 141.75(8) 6_656 2_665 ?
O2 Er1 O1 126.18(14) 6_656 6_657 ?
O1 Er1 Er1 37.76(9) 6_657 6_657 ?
O1 Er1 Er1 38.90(9) . 6_557 ?
O1 Er1 Er1 94.78(9) 6_657 6_557 ?
O1 Er1 Er1 171.44(9) . 6_657 ?
O1 Er1 O4 64.79(10) . 8_766 ?
O1 Er1 O4 144.74(8) . 5_766 ?
O1 Er1 O4 64.79(10) . 2_665 ?
O1 Er1 O4 144.74(8) . 3_756 ?
O1 Er1 O2 100.15(14) . 6_656 ?
O1 Er1 O1 133.68(11) . 6_657 ?
O1 Er1 O3 76.88(8) . 7_575 ?
O1 Er1 O3 76.88(8) . . ?
O3 Er1 Er1 106.31(7) 7_575 6_657 ?
O3 Er1 Er1 93.48(7) . 6_557 ?
O3 Er1 Er1 93.48(7) 7_575 6_557 ?
O3 Er1 Er1 106.31(7) . 6_657 ?
O3 Er1 O4 127.73(10) . 3_756 ?
O3 Er1 O4 71.71(10) . 2_665 ?
O3 Er1 O4 67.99(10) 7_575 3_756 ?
O3 Er1 O4 127.73(10) 7_575 5_766 ?
O3 Er1 O4 131.77(10) 7_575 2_665 ?
O3 Er1 O4 71.71(10) 7_575 8_766 ?
O3 Er1 O4 67.99(10) . 5_766 ?
O3 Er1 O4 131.77(10) . 8_766 ?
O3 Er1 O2 70.60(8) 7_575 6_656 ?
O3 Er1 O2 70.59(8) . 6_656 ?
O3 Er1 O1 115.48(8) . 6_657 ?
O3 Er1 O1 115.48(8) 7_575 6_657 ?
O3 Er1 O3 127.66(15) . 7_575 ?
Er1 O4 Er1 103.04(11) 5_766 2_664 ?
C2 O4 Er1 118.6(2) . 5_766 ?
C2 O4 Er1 138.3(2) . 2_664 ?
C1 O2 Er1 131.1(4) . 6_556 ?
Er1 O1 Er1 103.34(14) . 6_557 ?
C1 O1 Er1 121.8(3) . 6_557 ?
C1 O1 Er1 134.9(4) . . ?
C2 O3 Er1 118.3(3) . . ?
O2 C1 O1 126.7(5) . . ?
O2 C1 H1 116.6 . . ?
O1 C1 H1 116.6 . . ?
O4 C2 C2 114.9(4) . 5_766 ?
O3 C2 O4 126.3(4) . . ?
O3 C2 C2 118.9(5) . 5_766 ?

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 O4 C2 O3 -170.9(3) 5_766 . . . ?
Er1 O4 C2 O3 6.1(7) 2_664 . . . ?
Er1 O4 C2 C2 -173.9(3) 2_664 . . 5_766 ?
Er1 O4 C2 C2 9.0(5) 5_766 . . 5_766 ?
Er1 O2 C1 O1 180.000(0) 6_556 . . . ?
Er1 O1 C1 O2 0.000(1) . . . . ?
Er1 O1 C1 O2 180.000(1) 6_557 . . . ?
Er1 O3 C2 O4 -170.9(3) . . . . ?
Er1 O3 C2 C2 9.1(6) . . . 5_766 ?

_shelx_res_file                  
;
TITL 20_mf002_a.res in Pnma
    20_mf002.res
    created by SHELXL-2018/3 at 22:01:29 on 31-Mar-2021
REM Old TITL 20_MF002 in Pnma #62
REM SHELXT solution in Pnma
REM R1 0.025, Rweak 0.017, Alpha 0.015, Orientation as input
REM Formula found by SHELXT: C3 O6 Er
CELL 1.54184 6.919764 10.492097 6.533073 90 90 90
ZERR 4 0.000421 0.000643 0.000404 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Er O
UNIT 12 4 4 24

L.S. 80
PLAN  5
TEMP -153.15
CONF
BOND $H
LIST 6
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\20_MF002.hkl">
REM </olex2.extras>

WGHT    0.024500
FVAR       0.42917
ER1   3    0.799544    0.750000    0.633602    10.50000    0.00467    0.00530 =
         0.00266    0.00000    0.00022    0.00000
O4    4    0.910433    0.376020    0.350473    11.00000    0.00726    0.00810 =
         0.00624   -0.00105   -0.00133    0.00149
O2    4    0.446961    0.750000    0.196479    10.50000    0.01368    0.02290 =
         0.00785    0.00000   -0.00251    0.00000
O1    4    0.467770    0.750000    0.538316    10.50000    0.00785    0.00911 =
         0.00402    0.00000   -0.00102    0.00000
O3    4    0.758212    0.546378    0.478971    11.00000    0.00815    0.00587 =
         0.01595   -0.00260    0.00118   -0.00016
C1    1    0.376194    0.750000    0.368298    10.50000    0.00689    0.02004 =
         0.00416    0.00000    0.00099    0.00000
AFIX  43
H1    2    0.239102    0.750000    0.376081    10.50000   -1.20000
AFIX   0
C2    1    0.903191    0.479099    0.451913    11.00000    0.01034    0.01007 =
         0.00337   -0.00092   -0.00015    0.00072
HKLF 4




REM  20_mf002_a.res in Pnma
REM wR2 = 0.0430, GooF = S = 1.041, Restrained GooF = 1.041 for all data
REM R1 = 0.0190 for 447 Fo > 4sig(Fo) and 0.0217 for all 483 data
REM 52 parameters refined using 0 restraints

END

WGHT      0.0245      0.0000

REM Highest difference peak  0.681,  deepest hole -0.739,  1-sigma level  0.171
Q1    1   0.8050  0.6148  0.4938  11.00000  0.05    0.68
Q2    1   0.7691  0.7080  0.4219  11.00000  0.05    0.58
Q3    1   0.3144  0.7099  0.6509  11.00000  0.05    0.56
Q4    1   0.7120  0.3865  0.2808  11.00000  0.05    0.54
Q5    1   0.7134  0.5799  0.2412  11.00000  0.05    0.49
;
_shelx_res_checksum              99228
_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 1.837
_oxdiff_exptl_absorpt_empirical_full_min 0.785
