# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_06_gua04
_database_code_depnum_ccdc_archive 'CCDC 2320830'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_06_gua04            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.383 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and maximum completeness.
;
_vrf_PLAT974_06_gua04            
;
PROBLEM: Check Calcd Negative Resid. Density on       Er1      -1.55 eA-3
RESPONSE: No absorption correction applied, Er is a heavy element.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        06_GUA04
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   8.2526(2)
_cell_length_b                   6.54270(17)
_cell_length_c                   19.313(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1042.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2516
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.461
_cell_measurement_theta_min      2.128
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.753
_exptl_absorpt_coefficient_mu    2.925
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'Solvothermal synthesis,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.383
_diffrn_reflns_Laue_measured_fraction_max 0.241
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5059
_diffrn_reflns_point_group_measured_fraction_full 0.383
_diffrn_reflns_point_group_measured_fraction_max 0.241
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         25.461
_diffrn_reflns_theta_min         2.128
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.383
_diffrn_measured_fraction_theta_max 0.241
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                498
_reflns_number_total             734
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         734
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0223
_refine_ls_restrained_S_all      1.131
_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)+(0.0366P)²+0.2832P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0693
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-H1A
 0.88 with sigma of 0.02
 H1A_$1-C4
 2 with sigma of 0.2
 N1-H1A_$1 \\sim N2-H2A \\sim N2-H2B
 with sigma of 0.02
3. Restrained planarity
 O3, C3, O4, C3_$2, O3_$2, O4_$2
 with sigma of 0.1
 C4, N1, N2, N2_$1, H1A, H1A_$1, H2A, H2B, H2A_$1, H2B_$1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O2) = Uanis(C2)
Uanis(O4) = Uanis(C3) = Uanis(O3) = Uanis(C3) = Uanis(O3) = Uanis(O4)
5. Rigid body (RIGU) restrains
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
6.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.61637(3) 0.0220(4) Uani 1 2 d S T P . .
O2 O 0.2399(3) 0.8328(5) 0.6586(5) 0.045(4) Uani 1 1 d . . . . .
O4 O 0.5189(3) 0.3355(5) 0.4306(5) 0.036(3) Uani 1 1 d . . . . .
O1 O 0.4347(4) 0.5053(4) 0.7044(7) 0.0535(18) Uani 1 1 d . U . . .
O3 O 0.3537(3) 0.3174(5) 0.5204(4) 0.036(3) Uani 1 1 d . . . . .
C2 C 0.2500 1.0000 0.6296(8) 0.045(4) Uani 1 2 d S T P . .
H2 H 0.2500 1.0000 0.5814 0.054 Uiso 1 2 calc R U P . .
C3 C 0.4632(5) 0.3992(8) 0.4855(6) 0.036(3) Uani 1 1 d . . . . .
C1 C 0.5000 0.4176(11) 0.7500 0.040(2) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2755 0.7500 0.048 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.342(2) 0.056(3) Uani 1 2 d DS TU P . .
N1 N 0.2500 1.0000 0.409(2) 0.094(5) Uani 1 2 d DS TU P . .
H1A H 0.206(8) 0.932(13) 0.443(4) 0.112 Uiso 1 1 d D U . . .
N2 N 0.3382(5) 1.1327(6) 0.3077(7) 0.075(8) Uani 1 1 d D . . . .
H2A H 0.3964 1.2203 0.3297 0.090 Uiso 1 1 calc DR U . . .
H2B H 0.3377 1.1320 0.2632 0.090 Uiso 1 1 calc DR U . . .


_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 O2 2.327(5) . ?
Er1 O2 2.327(5) 2_565 ?
Er1 O4 2.371(4) 6_556 ?
Er1 O4 2.371(4) 5_666 ?
Er1 O1 2.284(10) . ?
Er1 O1 2.284(10) 2_565 ?
Er1 O3 2.366(6) 2_565 ?
Er1 O3 2.366(6) . ?
O2 C2 1.232(9) . ?
O4 Er1 2.371(4) 5_666 ?
O4 C3 1.229(12) . ?
O1 C1 1.181(10) . ?
O3 C3 1.247(8) . ?
C2 O2 1.232(9) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.556(13) 5_666 ?
C1 O1 1.181(10) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.28(7) . ?
C4 N2 1.31(2) 2_575 ?
C4 N2 1.31(2) . ?
N1 H1A 0.872(14) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 139.0(5) . 2_565 ?
O2 Er1 O4 122.01(12) . 6_556 ?
O2 Er1 O4 74.82(19) 2_565 6_556 ?
O2 Er1 O4 122.01(12) 2_565 5_666 ?
O2 Er1 O4 74.82(19) . 5_666 ?
O2 Er1 O3 77.8(3) . 2_565 ?
O2 Er1 O3 139.5(2) 2_565 2_565 ?
O2 Er1 O3 77.8(3) 2_565 . ?
O2 Er1 O3 139.5(2) . . ?
O4 Er1 O4 135.0(4) 5_666 6_556 ?
O1 Er1 O2 75.45(19) . . ?
O1 Er1 O2 74.3(2) . 2_565 ?
O1 Er1 O2 75.45(19) 2_565 2_565 ?
O1 Er1 O2 74.3(2) 2_565 . ?
O1 Er1 O4 75.0(3) 2_565 6_556 ?
O1 Er1 O4 146.0(2) . 6_556 ?
O1 Er1 O4 146.0(2) 2_565 5_666 ?
O1 Er1 O4 75.0(3) . 5_666 ?
O1 Er1 O1 83.8(5) 2_565 . ?
O1 Er1 O3 110.5(2) 2_565 2_565 ?
O1 Er1 O3 144.81(15) 2_565 . ?
O1 Er1 O3 110.5(2) . . ?
O1 Er1 O3 144.81(15) . 2_565 ?
O3 Er1 O4 68.79(18) . 5_666 ?
O3 Er1 O4 76.23(19) 2_565 5_666 ?
O3 Er1 O4 76.23(19) . 6_556 ?
O3 Er1 O4 68.79(18) 2_565 6_556 ?
O3 Er1 O3 76.8(3) 2_565 . ?
C2 O2 Er1 132.0(9) . . ?
C3 O4 Er1 118.5(3) . 5_666 ?
C1 O1 Er1 148.4(4) . . ?
C3 O3 Er1 117.9(4) . . ?
O2 C2 O2 125.9(15) . 2_575 ?
O2 C2 H2 117.1 . . ?
O2 C2 H2 117.1 2_575 . ?
O4 C3 O3 126.2(6) . . ?
O4 C3 C3 116.9(8) . 5_666 ?
O3 C3 C3 116.9(11) . 5_666 ?
O1 C1 O1 121.8(9) . 3_656 ?
O1 C1 H1 119.1 3_656 . ?
O1 C1 H1 119.1 . . ?
N1 C4 N2 120.4(16) . . ?
N1 C4 N2 120.4(16) . 2_575 ?
N2 C4 N2 119(3) 2_575 . ?
C4 N1 H1A 139(9) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -171.7(3) . . . 2_575 ?
Er1 O4 C3 O3 -172.1(5) 5_666 . . . ?
Er1 O4 C3 C3 7.7(10) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -159.8(14) . . . 3_656 ?
Er1 O3 C3 O4 -172.2(6) . . . . ?
Er1 O3 C3 C3 7.9(9) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 06_GUA04
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_07_gua04
_database_code_depnum_ccdc_archive 'CCDC 2320832'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_07_gua04            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.381 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        07_GUA04
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   8.1956(2)
_cell_length_b                   6.53400(18)
_cell_length_c                   19.322(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1034.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2326
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.972
_cell_measurement_theta_min      2.131
_shelx_estimated_absorpt_T_max   0.894
_shelx_estimated_absorpt_T_min   0.678
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'Solvothermal synthesis,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.039
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.381
_diffrn_reflns_Laue_measured_fraction_max 0.231
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4932
_diffrn_reflns_point_group_measured_fraction_full 0.381
_diffrn_reflns_point_group_measured_fraction_max 0.231
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         25.972
_diffrn_reflns_theta_min         2.131
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.381
_diffrn_measured_fraction_theta_max 0.231
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                484
_reflns_number_total             737
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         737
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0279
_refine_ls_restrained_S_all      1.130
_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)+(0.0421P)²+1.0904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0865
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-H1A
 0.88 with sigma of 0.02
 C4-H1A
 2 with sigma of 0.02
 N1-H1A \\sim N2-H2A \\sim N2-H2B
 with sigma of 0.02
3. Restrained planarity
 O3, C3, O4, C3_$2, O3_$2, O4_$2
 with sigma of 0.1
 C4, H1A, N1, H1A_$1, N2, N2_$1, H2A, H2B, H2A_$1, H2B_$1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O2) = Uanis(C2)
Uanis(O4) = Uanis(C3) = Uanis(O3) = Uanis(C3) = Uanis(O3) = Uanis(O4)
5. Rigid body (RIGU) restrains
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
6.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.61647(4) 0.0254(6) Uani 1 2 d S T P . .
O2 O 0.2406(5) 0.8329(7) 0.6586(7) 0.040(5) Uani 1 1 d . . . . .
O4 O 0.5176(5) 0.3365(7) 0.4315(7) 0.044(4) Uani 1 1 d . . . . .
O1 O 0.4358(6) 0.5043(6) 0.7031(10) 0.060(2) Uani 1 1 d . U . . .
O3 O 0.3531(5) 0.3166(7) 0.5204(6) 0.044(4) Uani 1 1 d . . . . .
C2 C 0.2500 1.0000 0.6293(11) 0.040(5) Uani 1 2 d S T P . .
H2 H 0.2500 1.0000 0.5812 0.048 Uiso 1 2 calc R U P . .
C3 C 0.4623(7) 0.4001(11) 0.4861(7) 0.044(4) Uani 1 1 d . . . . .
C1 C 0.5000 0.4160(16) 0.7500 0.046(3) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2737 0.7500 0.056 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.3416(15) 0.058(4) Uani 1 2 d DS TU P . .
N1 N 0.2500 1.0000 0.408(3) 0.088(5) Uani 1 2 d DS TU P . .
H1A H 0.203(8) 0.928(11) 0.440(3) 0.105 Uiso 1 1 d D U . . .
N2 N 0.3381(7) 1.1330(9) 0.3081(9) 0.074(11) Uani 1 1 d D . . . .
H2A H 0.3961 1.2205 0.3305 0.089 Uiso 1 1 calc DR U . . .
H2B H 0.3383 1.1333 0.2636 0.089 Uiso 1 1 calc DR U . . .


_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 O2 2.324(7) 2_565 ?
Er1 O2 2.324(7) . ?
Er1 O4 2.372(6) 5_666 ?
Er1 O4 2.372(6) 6_556 ?
Er1 O1 2.264(13) . ?
Er1 O1 2.264(13) 2_565 ?
Er1 O3 2.366(9) 2_565 ?
Er1 O3 2.366(9) . ?
O2 C2 1.232(12) . ?
O4 Er1 2.372(6) 5_666 ?
O4 C3 1.221(16) . ?
O1 C1 1.196(14) . ?
O3 C3 1.240(11) . ?
C2 O2 1.232(12) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.541(18) 5_666 ?
C1 O1 1.196(14) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.28(6) . ?
C4 N2 1.303(16) 2_575 ?
C4 N2 1.303(16) . ?
N1 H1A 0.873(14) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 139.0(6) 2_565 . ?
O2 Er1 O4 122.14(17) . 6_556 ?
O2 Er1 O4 122.14(17) 2_565 5_666 ?
O2 Er1 O4 75.0(3) 2_565 6_556 ?
O2 Er1 O4 75.0(3) . 5_666 ?
O2 Er1 O3 139.6(3) 2_565 2_565 ?
O2 Er1 O3 77.8(4) 2_565 . ?
O2 Er1 O3 139.6(3) . . ?
O2 Er1 O3 77.8(4) . 2_565 ?
O4 Er1 O4 134.0(6) 5_666 6_556 ?
O1 Er1 O2 75.6(3) . . ?
O1 Er1 O2 75.6(3) 2_565 2_565 ?
O1 Er1 O2 74.3(3) . 2_565 ?
O1 Er1 O2 74.3(3) 2_565 . ?
O1 Er1 O4 75.1(4) 2_565 6_556 ?
O1 Er1 O4 146.6(3) 2_565 5_666 ?
O1 Er1 O4 146.6(3) . 6_556 ?
O1 Er1 O4 75.1(4) . 5_666 ?
O1 Er1 O1 84.6(7) 2_565 . ?
O1 Er1 O3 110.3(4) . . ?
O1 Er1 O3 144.5(2) . 2_565 ?
O1 Er1 O3 144.5(2) 2_565 . ?
O1 Er1 O3 110.3(4) 2_565 2_565 ?
O3 Er1 O4 75.7(3) 2_565 5_666 ?
O3 Er1 O4 68.6(3) 2_565 6_556 ?
O3 Er1 O4 75.7(3) . 6_556 ?
O3 Er1 O4 68.6(3) . 5_666 ?
O3 Er1 O3 76.6(4) 2_565 . ?
C2 O2 Er1 131.8(13) . . ?
C3 O4 Er1 118.8(5) . 5_666 ?
C1 O1 Er1 148.2(5) . . ?
C3 O3 Er1 117.0(6) . . ?
O2 C2 O2 125(2) . 2_575 ?
O2 C2 H2 117.3 . . ?
O2 C2 H2 117.3 2_575 . ?
O4 C3 O3 125.5(8) . . ?
O4 C3 C3 116.2(10) . 5_666 ?
O3 C3 C3 118.4(14) . 5_666 ?
O1 C1 O1 122.3(12) . 3_656 ?
O1 C1 H1 118.9 . . ?
O1 C1 H1 118.9 3_656 . ?
N1 C4 N2 119.8(12) . . ?
N1 C4 N2 119.8(12) . 2_575 ?
N2 C4 N2 120(2) 2_575 . ?
C4 N1 H1A 136(9) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -172.4(4) . . . 2_575 ?
Er1 O4 C3 O3 -171.9(6) 5_666 . . . ?
Er1 O4 C3 C3 7.4(13) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -156(2) . . . 3_656 ?
Er1 O3 C3 O4 -172.5(8) . . . . ?
Er1 O3 C3 C3 8.2(11) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 07_GUA04
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_12_gua03
_database_code_depnum_ccdc_archive 'CCDC 2320831'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_12_gua03            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.483 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum completeness.
;
_vrf_PLAT974_12_gua03            
;
PROBLEM: Check Calcd Negative Resid. Density on       Er1      -2.51 eA-3
RESPONSE: No absorption correction applied, Er is a heavy element.
;
_vrf_PLAT911_12_gua03            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        280 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        12_GUA03
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   8.45510(13)
_cell_length_b                   6.58400(7)
_cell_length_c                   19.2134(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1069.58(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3050
_cell_measurement_temperature    300
_cell_measurement_theta_max      26.532
_cell_measurement_theta_min      2.115
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.758
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.518
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'solvothermal synthesis.,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.483
_diffrn_reflns_Laue_measured_fraction_max 0.282
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5151
_diffrn_reflns_point_group_measured_fraction_full 0.483
_diffrn_reflns_point_group_measured_fraction_max 0.282
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         26.532
_diffrn_reflns_theta_min         2.115
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.483
_diffrn_measured_fraction_theta_max 0.282
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                670
_reflns_number_total             986
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         986
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0180
_refine_ls_restrained_S_all      1.083
_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)+(0.0262P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0528
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-H1A
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) = Uanis(C2)
4. Rigid body (RIGU) restrains
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.61608(2) 0.01626(17) Uani 1 2 d S T P . .
O2 O 0.23872(18) 0.8332(3) 0.6579(3) 0.0327(17) Uani 1 1 d . . . . .
O4 O 0.5237(2) 0.3329(3) 0.4313(3) 0.038(2) Uani 1 1 d . . . . .
O1 O 0.4325(3) 0.5080(2) 0.7028(4) 0.0427(18) Uani 1 1 d . U . . .
O3 O 0.3552(2) 0.3204(2) 0.5200(2) 0.0356(19) Uani 1 1 d . . . . .
C2 C 0.2500 1.0000 0.6273(4) 0.0327(17) Uani 1 2 d S T P . .
H2 H 0.2500 1.0000 0.5789 0.039 Uiso 1 2 calc R U P . .
C3 C 0.4655(4) 0.3993(5) 0.4846(4) 0.029(3) Uani 1 1 d . . . . .
C1 C 0.5000 0.4230(6) 0.7500 0.030(2) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2817 0.7500 0.036 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.3444(13) 0.057(4) Uani 1 2 d S TU P . .
N1 N 0.2500 1.0000 0.4093(14) 0.099(6) Uani 1 2 d DS TU P . .
H1A H 0.291(7) 1.082(10) 0.442(3) 0.119 Uiso 1 1 d D U . . .
N2 N 0.3371(3) 1.1304(4) 0.3097(4) 0.061(3) Uani 1 1 d . . . . .
H2A H 0.3948 1.2167 0.3316 0.073 Uiso 1 1 calc R U . . .
H2B H 0.3364 1.1294 0.2649 0.073 Uiso 1 1 calc R U . . .


_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 O2 2.338(3) 2_565 ?
Er1 O2 2.338(3) . ?
Er1 O4 2.388(2) 6_556 ?
Er1 O4 2.388(2) 5_666 ?
Er1 O1 2.271(5) 2_565 ?
Er1 O1 2.271(5) . ?
Er1 O3 2.366(3) . ?
Er1 O3 2.366(3) 2_565 ?
O2 C2 1.250(5) . ?
O4 Er1 2.388(2) 5_666 ?
O4 C3 1.216(7) . ?
O1 C1 1.209(5) . ?
O3 C3 1.266(5) . ?
C2 O2 1.250(5) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.565(8) 5_666 ?
C1 O1 1.209(5) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.25(4) . ?
C4 N2 1.314(13) 2_575 ?
C4 N2 1.314(13) . ?
N1 H1A 0.89(2) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 139.8(3) 2_565 . ?
O2 Er1 O4 74.43(10) . 5_666 ?
O2 Er1 O4 74.43(10) 2_565 6_556 ?
O2 Er1 O4 122.04(7) 2_565 5_666 ?
O2 Er1 O4 122.04(7) . 6_556 ?
O2 Er1 O3 77.52(14) 2_565 . ?
O2 Er1 O3 138.79(12) 2_565 2_565 ?
O2 Er1 O3 77.52(14) . 2_565 ?
O2 Er1 O3 138.79(12) . . ?
O4 Er1 O4 135.1(2) 6_556 5_666 ?
O1 Er1 O2 75.05(11) 2_565 . ?
O1 Er1 O2 75.05(11) . 2_565 ?
O1 Er1 O2 75.76(11) 2_565 2_565 ?
O1 Er1 O2 75.76(11) . . ?
O1 Er1 O4 74.03(16) . 5_666 ?
O1 Er1 O4 146.60(13) . 6_556 ?
O1 Er1 O4 146.60(13) 2_565 5_666 ?
O1 Er1 O4 74.03(16) 2_565 6_556 ?
O1 Er1 O1 85.6(3) . 2_565 ?
O1 Er1 O3 109.20(14) 2_565 2_565 ?
O1 Er1 O3 144.70(8) 2_565 . ?
O1 Er1 O3 144.70(8) . 2_565 ?
O1 Er1 O3 109.20(14) . . ?
O3 Er1 O4 76.89(11) . 6_556 ?
O3 Er1 O4 68.36(9) . 5_666 ?
O3 Er1 O4 76.89(11) 2_565 5_666 ?
O3 Er1 O4 68.36(9) 2_565 6_556 ?
O3 Er1 O3 77.40(16) . 2_565 ?
C2 O2 Er1 131.3(5) . . ?
C3 O4 Er1 118.6(2) . 5_666 ?
C1 O1 Er1 149.3(2) . . ?
C3 O3 Er1 119.4(3) . . ?
O2 C2 O2 123.8(8) 2_575 . ?
O2 C2 H2 118.1 2_575 . ?
O2 C2 H2 118.1 . . ?
O4 C3 O3 127.1(3) . . ?
O4 C3 C3 118.2(5) . 5_666 ?
O3 C3 C3 114.7(7) . 5_666 ?
O1 C1 O1 124.8(5) 3_656 . ?
O1 C1 H1 117.6 3_656 . ?
O1 C1 H1 117.6 . . ?
N1 C4 N2 120.6(10) . . ?
N1 C4 N2 120.6(10) . 2_575 ?
N2 C4 N2 119(2) 2_575 . ?
C4 N1 H1A 134(6) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -170.67(16) . . . 2_575 ?
Er1 O4 C3 O3 -173.3(3) 5_666 . . . ?
Er1 O4 C3 C3 4.8(8) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -158.9(8) . . . 3_656 ?
Er1 O3 C3 O4 -174.5(5) . . . . ?
Er1 O3 C3 C3 7.4(6) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 
'in diamond anvil cell, with pressure transmitting medium  of 4:1 methaol:ethanol.'
_olex2_submission_original_sample_id 12_GUA03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_32_gua03
_database_code_depnum_ccdc_archive 'CCDC 2320833'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT088_32_gua03            
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.97 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT342_32_gua03            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.
RESPONSE: A combination of heavy and light elements is present in the structure, and only a single C-C bond is present.
;
_vrf_PLAT911_32_gua03            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        196 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        32_GUA03
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   7.8462(14)
_cell_length_b                   6.5142(11)
_cell_length_c                   19.58(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1000.6(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2269
_cell_measurement_temperature    300
_cell_measurement_theta_max      16.972
_cell_measurement_theta_min      2.137
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.744
_exptl_absorpt_coefficient_mu    3.048
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.691
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'Solvothermal synthesis,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.511
_diffrn_reflns_Laue_measured_fraction_max 0.512
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2932
_diffrn_reflns_point_group_measured_fraction_full 0.511
_diffrn_reflns_point_group_measured_fraction_max 0.512
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         16.972
_diffrn_reflns_theta_min         2.137
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.511
_diffrn_measured_fraction_theta_max 0.512
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                212
_reflns_number_total             472
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         472
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      0.826
_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)+(0.0608P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1058
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Restrained distances
 N1-H1A
 0.9 with sigma of 0.05
 H1A-C4
 2 with sigma of 0.05
3. Restrained planarity
 O4_$1, O3, C3, O4, C3_$1, O3_$1
 with sigma of 0.1
 N1, C4, N2, H1A, H2A, H2B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) = Uanis(O2)
5. Rigid body (RIGU) restrains
 O2, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, C3, O4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
6.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.61681(11) 0.0512(9) Uani 1 2 d S T P . .
O2 O 0.2433(13) 0.8349(12) 0.6534(11) 0.053(3) Uani 1 1 d . U . . .
O4 O 0.5130(16) 0.338(2) 0.4334(15) 0.095(8) Uani 1 1 d . U . . .
O1 O 0.4458(16) 0.4986(16) 0.7023(16) 0.081(5) Uani 1 1 d . U . . .
O3 O 0.3495(17) 0.3160(17) 0.5240(14) 0.091(8) Uani 1 1 d . U . . .
C2 C 0.2500 1.0000 0.6272(19) 0.053(3) Uani 1 2 d S TU P . .
H2 H 0.2500 1.0000 0.5797 0.063 Uiso 1 2 calc R U P . .
C3 C 0.4589(19) 0.389(3) 0.4850(12) 0.060(8) Uani 1 1 d . U . . .
C1 C 0.5000 0.395(5) 0.7500 0.067(8) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2519 0.7500 0.080 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.342(3) 0.069(8) Uani 1 2 d DS TU P . .
N1 N 0.2500 1.0000 0.407(4) 0.113(11) Uani 1 2 d DS TU P . .
N2 N 0.3362(19) 1.136(3) 0.3015(17) 0.102(9) Uani 1 1 d . U . . .
H2A H 0.3965 1.2317 0.3200 0.123 Uiso 1 1 calc R U . . .
H2B H 0.3303 1.1270 0.2577 0.123 Uiso 1 1 calc R U . . .
H1A H 0.317(11) 1.091(17) 0.434(5) 0.123 Uiso 1 1 d D U . . .


_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 O2 2.297(9) 2_565 ?
Er1 O2 2.297(9) . ?
Er1 O4 2.353(16) 6_556 ?
Er1 O4 2.353(16) 5_666 ?
Er1 O1 2.27(2) . ?
Er1 O1 2.27(2) 2_565 ?
Er1 O3 2.31(2) . ?
Er1 O3 2.31(2) 2_565 ?
O2 C2 1.19(2) . ?
O4 Er1 2.353(16) 5_666 ?
O4 C3 1.14(3) . ?
O1 C1 1.23(2) . ?
O3 C3 1.24(3) . ?
C2 O2 1.19(2) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.69(4) 5_666 ?
C1 O1 1.23(2) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.27(9) . ?
C4 N2 1.37(3) 2_575 ?
C4 N2 1.37(3) . ?
N1 H1A 0.96(5) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 143.6(10) 2_565 . ?
O2 Er1 O4 73.9(6) . 5_666 ?
O2 Er1 O4 73.9(6) 2_565 6_556 ?
O2 Er1 O4 122.5(5) 2_565 5_666 ?
O2 Er1 O4 122.5(5) . 6_556 ?
O2 Er1 O3 75.2(6) 2_565 . ?
O2 Er1 O3 138.2(6) 2_565 2_565 ?
O2 Er1 O3 75.2(6) . 2_565 ?
O2 Er1 O3 138.2(6) . . ?
O4 Er1 O4 130.6(13) 6_556 5_666 ?
O1 Er1 O2 77.9(5) . . ?
O1 Er1 O2 77.8(5) 2_565 2_565 ?
O1 Er1 O2 75.6(5) . 2_565 ?
O1 Er1 O2 75.6(5) 2_565 . ?
O1 Er1 O4 147.2(7) 2_565 5_666 ?
O1 Er1 O4 77.0(8) 2_565 6_556 ?
O1 Er1 O4 77.0(8) . 5_666 ?
O1 Er1 O4 147.2(7) . 6_556 ?
O1 Er1 O1 85.1(13) 2_565 . ?
O1 Er1 O3 144.0(5) . 2_565 ?
O1 Er1 O3 110.4(8) . . ?
O1 Er1 O3 110.4(7) 2_565 2_565 ?
O1 Er1 O3 144.0(5) 2_565 . ?
O3 Er1 O4 72.9(7) . 6_556 ?
O3 Er1 O4 68.7(6) . 5_666 ?
O3 Er1 O4 72.9(7) 2_565 5_666 ?
O3 Er1 O4 68.7(6) 2_565 6_556 ?
O3 Er1 O3 76.4(11) . 2_565 ?
C2 O2 Er1 136(2) . . ?
C3 O4 Er1 122.3(17) . 5_666 ?
C1 O1 Er1 142.7(16) . . ?
C3 O3 Er1 121.2(14) . . ?
O2 C2 O2 129(4) . 2_575 ?
O2 C2 H2 115.5 . . ?
O2 C2 H2 115.5 2_575 . ?
O4 C3 O3 134(2) . . ?
O4 C3 C3 114(2) . 5_666 ?
O3 C3 C3 112(3) . 5_666 ?
O1 C1 O1 113(4) . 3_656 ?
O1 C1 H1 123.4 . . ?
O1 C1 H1 123.4 3_656 . ?
N1 C4 N2 125(2) . . ?
N1 C4 N2 125(2) . 2_575 ?
N2 C4 N2 110(5) 2_575 . ?
C4 N1 H1A 124(10) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -174.3(11) . . . 2_575 ?
Er1 O4 C3 O3 -171.4(14) 5_666 . . . ?
Er1 O4 C3 C3 10.0(19) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -149(3) . . . 3_656 ?
Er1 O3 C3 O4 -170.3(16) . . . . ?
Er1 O3 C3 C3 8.4(18) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 methanol:ethanol'
_olex2_submission_original_sample_id 32_GUA03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_30_gua03
_database_code_depnum_ccdc_archive 'CCDC 2320835'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_30_gua03            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.484 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness..
;
_vrf_PLAT911_30_gua03            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        273 Report
RESPONSE: limited accessibility to reciprocal space.
;
_vrf_PLAT974_30_gua03            
;
PROBLEM: Check Calcd Negative Resid. Density on       Er1      -1.82 eA-3
RESPONSE: no absorption correction applied, Er is a heavy element.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        30_GUA03
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   8.3154(2)
_cell_length_b                   6.54900(9)
_cell_length_c                   19.234(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1047.43(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2780
_cell_measurement_temperature    300
_cell_measurement_theta_max      26.690
_cell_measurement_theta_min      2.126
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.754
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.571
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'Solvothermal synthesis,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.484
_diffrn_reflns_Laue_measured_fraction_max 0.284
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5077
_diffrn_reflns_point_group_measured_fraction_full 0.484
_diffrn_reflns_point_group_measured_fraction_max 0.284
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         26.690
_diffrn_reflns_theta_min         2.126
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.484
_diffrn_measured_fraction_theta_max 0.284
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                659
_reflns_number_total             988
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         988
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0273
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0616P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0948
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-H1A
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) = Uanis(C2)
4. Rigid body (RIGU) restrains
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.61625(3) 0.0226(3) Uani 1 2 d S T P . .
O2 O 0.2398(3) 0.8337(5) 0.6578(5) 0.042(3) Uani 1 1 d . . . . .
O4 O 0.5214(4) 0.3338(4) 0.4311(4) 0.057(3) Uani 1 1 d . . . . .
O1 O 0.4351(5) 0.5056(3) 0.7026(6) 0.060(2) Uani 1 1 d . U . . .
O3 O 0.3538(3) 0.3176(3) 0.5204(3) 0.048(3) Uani 1 1 d . . . . .
C2 C 0.2500 1.0000 0.6282(7) 0.042(3) Uani 1 2 d S T P . .
H2 H 0.2500 1.0000 0.5798 0.050 Uiso 1 2 calc R U P . .
C3 C 0.4644(6) 0.3987(7) 0.4860(6) 0.042(5) Uani 1 1 d . . . . .
C1 C 0.5000 0.4200(10) 0.7500 0.043(3) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2779 0.7500 0.052 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.345(2) 0.062(5) Uani 1 2 d S TU P . .
N1 N 0.2500 1.0000 0.411(2) 0.108(8) Uani 1 2 d DS TU P . .
H1A H 0.308(11) 1.066(16) 0.443(5) 0.130 Uiso 1 1 d D U . . .
N2 N 0.3380(5) 1.1314(5) 0.3086(6) 0.079(5) Uani 1 1 d . . . . .
H2A H 0.3969 1.2193 0.3300 0.095 Uiso 1 1 calc R U . . .
H2B H 0.3363 1.1289 0.2639 0.095 Uiso 1 1 calc R U . . .


_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 O2 2.328(5) . ?
Er1 O2 2.328(5) 2_565 ?
Er1 O4 2.372(4) 6_556 ?
Er1 O4 2.372(4) 5_666 ?
Er1 O1 2.264(9) 2_565 ?
Er1 O1 2.264(9) . ?
Er1 O3 2.361(5) . ?
Er1 O3 2.361(5) 2_565 ?
O2 C2 1.232(8) . ?
O4 Er1 2.372(4) 5_666 ?
O4 C3 1.233(12) . ?
O1 C1 1.199(9) . ?
O3 C3 1.251(8) . ?
C2 O2 1.232(8) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.549(12) 5_666 ?
C1 O1 1.199(9) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.28(6) . ?
C4 N2 1.32(2) . ?
C4 N2 1.33(2) 2_575 ?
N1 H1A 0.88(2) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 139.9(5) . 2_565 ?
O2 Er1 O4 122.21(12) 2_565 5_666 ?
O2 Er1 O4 122.21(12) . 6_556 ?
O2 Er1 O4 74.37(17) . 5_666 ?
O2 Er1 O4 74.37(17) 2_565 6_556 ?
O2 Er1 O3 139.1(2) . . ?
O2 Er1 O3 77.3(2) . 2_565 ?
O2 Er1 O3 139.1(2) 2_565 2_565 ?
O2 Er1 O3 77.3(2) 2_565 . ?
O4 Er1 O4 134.8(4) 6_556 5_666 ?
O1 Er1 O2 75.99(19) 2_565 2_565 ?
O1 Er1 O2 76.00(19) . . ?
O1 Er1 O2 74.87(19) 2_565 . ?
O1 Er1 O2 74.86(19) . 2_565 ?
O1 Er1 O4 74.3(3) . 5_666 ?
O1 Er1 O4 146.5(2) . 6_556 ?
O1 Er1 O4 146.5(2) 2_565 5_666 ?
O1 Er1 O4 74.3(3) 2_565 6_556 ?
O1 Er1 O1 85.7(5) . 2_565 ?
O1 Er1 O3 109.4(2) 2_565 2_565 ?
O1 Er1 O3 144.41(14) 2_565 . ?
O1 Er1 O3 144.40(14) . 2_565 ?
O1 Er1 O3 109.4(2) . . ?
O3 Er1 O4 76.16(17) . 6_556 ?
O3 Er1 O4 68.84(15) . 5_666 ?
O3 Er1 O4 76.16(17) 2_565 5_666 ?
O3 Er1 O4 68.84(15) 2_565 6_556 ?
O3 Er1 O3 77.3(2) . 2_565 ?
C2 O2 Er1 132.0(8) . . ?
C3 O4 Er1 118.6(3) . 5_666 ?
C1 O1 Er1 148.9(3) . . ?
C3 O3 Er1 117.8(4) . . ?
O2 C2 O2 125.0(13) . 2_575 ?
O2 C2 H2 117.5 . . ?
O2 C2 H2 117.5 2_575 . ?
O4 C3 O3 126.1(5) . . ?
O4 C3 C3 116.4(8) . 5_666 ?
O3 C3 C3 117.5(11) . 5_666 ?
O1 C1 O1 124.2(7) 3_656 . ?
O1 C1 H1 117.9 3_656 . ?
O1 C1 H1 117.9 . . ?
N1 C4 N2 121.5(15) . 2_575 ?
N1 C4 N2 121.5(15) . . ?
N2 C4 N2 117(3) . 2_575 ?
C4 N1 H1A 133(9) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -171.5(2) . . . 2_575 ?
Er1 O4 C3 O3 -173.4(5) 5_666 . . . ?
Er1 O4 C3 C3 7.6(12) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -155.9(14) . . . 3_656 ?
Er1 O3 C3 O4 -172.8(7) . . . . ?
Er1 O3 C3 C3 6.3(10) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 30_GUA03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_24_gua03
_database_code_depnum_ccdc_archive 'CCDC 2320838'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_24_gua03            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.468 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness..
;
_vrf_PLAT911_24_gua03            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        291 Report
RESPONSE: limited accessibility to reciprocal space.
;
_vrf_PLAT974_24_gua03            
;
PROBLEM: Check Calcd Negative Resid. Density on       Er1      -1.95 eA-3
RESPONSE: no absorption correction applied, Er is a heavy element.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        24_GUA03
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   8.35830(18)
_cell_length_b                   6.55850(8)
_cell_length_c                   19.218(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1053.47(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2898
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.646
_cell_measurement_theta_min      2.123
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.755
_exptl_absorpt_coefficient_mu    2.895
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.556
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'Solvothermal synthesis,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooled'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.468
_diffrn_reflns_Laue_measured_fraction_max 0.311
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5142
_diffrn_reflns_point_group_measured_fraction_full 0.468
_diffrn_reflns_point_group_measured_fraction_max 0.311
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         25.646
_diffrn_reflns_theta_min         2.123
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.468
_diffrn_measured_fraction_theta_max 0.311
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                597
_reflns_number_total             971
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         971
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0207
_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)+(0.0322P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0623
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-H1A
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) = Uanis(C2)
4. Rigid body (RIGU) restrains
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.61617(2) 0.0207(2) Uani 1 2 d S T P . .
O2 O 0.2399(3) 0.8329(4) 0.6577(4) 0.034(2) Uani 1 1 d . . . . .
O4 O 0.5225(3) 0.3333(4) 0.4318(4) 0.050(3) Uani 1 1 d . . . . .
O1 O 0.4344(4) 0.5061(3) 0.7023(5) 0.055(2) Uani 1 1 d . U . . .
O3 O 0.3542(3) 0.3184(3) 0.5195(3) 0.045(2) Uani 1 1 d . . . . .
C2 C 0.2500 1.0000 0.6286(5) 0.034(2) Uani 1 2 d S T P . .
H2 H 0.2500 1.0000 0.5802 0.041 Uiso 1 2 calc R U P . .
C3 C 0.4642(5) 0.3982(6) 0.4856(5) 0.036(4) Uani 1 1 d . . . . .
C1 C 0.5000 0.4201(9) 0.7500 0.038(2) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2783 0.7500 0.046 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.3452(16) 0.065(4) Uani 1 2 d S TU P . .
N1 N 0.2500 1.0000 0.411(2) 0.119(7) Uani 1 2 d DS TU P . .
H1A H 0.297(10) 1.082(14) 0.443(4) 0.143 Uiso 1 1 d D U . . .
N2 N 0.3369(5) 1.1306(5) 0.3089(5) 0.077(5) Uani 1 1 d . . . . .
H2A H 0.3955 1.2188 0.3300 0.092 Uiso 1 1 calc R U . . .
H2B H 0.3347 1.1274 0.2642 0.092 Uiso 1 1 calc R U . . .


_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 O2 2.326(3) 2_565 ?
Er1 O2 2.326(3) . ?
Er1 O4 2.379(3) 6_556 ?
Er1 O4 2.379(3) 5_666 ?
Er1 O1 2.262(7) . ?
Er1 O1 2.262(7) 2_565 ?
Er1 O3 2.372(4) . ?
Er1 O3 2.372(4) 2_565 ?
O2 C2 1.233(5) . ?
O4 Er1 2.379(3) 5_666 ?
O4 C3 1.220(10) . ?
O1 C1 1.208(7) . ?
O3 C3 1.243(7) . ?
C2 O2 1.233(5) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.564(10) 5_666 ?
C1 O1 1.208(7) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.27(5) . ?
C4 N2 1.322(17) . ?
C4 N2 1.322(17) 2_575 ?
N1 H1A 0.90(2) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 139.9(3) 2_565 . ?
O2 Er1 O4 74.38(14) . 5_666 ?
O2 Er1 O4 74.38(14) 2_565 6_556 ?
O2 Er1 O4 122.36(10) 2_565 5_666 ?
O2 Er1 O4 122.36(10) . 6_556 ?
O2 Er1 O3 77.53(18) 2_565 . ?
O2 Er1 O3 138.87(16) 2_565 2_565 ?
O2 Er1 O3 77.53(18) . 2_565 ?
O2 Er1 O3 138.87(16) . . ?
O4 Er1 O4 134.4(3) 6_556 5_666 ?
O1 Er1 O2 75.94(14) . . ?
O1 Er1 O2 75.94(14) 2_565 2_565 ?
O1 Er1 O2 74.98(14) . 2_565 ?
O1 Er1 O2 74.98(14) 2_565 . ?
O1 Er1 O4 146.75(17) 2_565 5_666 ?
O1 Er1 O4 74.4(2) 2_565 6_556 ?
O1 Er1 O4 74.4(2) . 5_666 ?
O1 Er1 O4 146.75(17) . 6_556 ?
O1 Er1 O1 85.9(4) 2_565 . ?
O1 Er1 O3 144.51(11) . 2_565 ?
O1 Er1 O3 109.37(19) . . ?
O1 Er1 O3 109.37(19) 2_565 2_565 ?
O1 Er1 O3 144.51(11) 2_565 . ?
O3 Er1 O4 76.07(15) . 6_556 ?
O3 Er1 O4 68.53(13) . 5_666 ?
O3 Er1 O4 76.07(15) 2_565 5_666 ?
O3 Er1 O4 68.53(13) 2_565 6_556 ?
O3 Er1 O3 76.9(2) . 2_565 ?
C2 O2 Er1 132.6(5) . . ?
C3 O4 Er1 119.2(3) . 5_666 ?
C1 O1 Er1 148.9(3) . . ?
C3 O3 Er1 118.1(4) . . ?
O2 C2 O2 126.2(9) 2_575 . ?
O2 C2 H2 116.9 2_575 . ?
O2 C2 H2 116.9 . . ?
O4 C3 O3 126.4(5) . . ?
O4 C3 C3 116.4(7) . 5_666 ?
O3 C3 C3 117.2(9) . 5_666 ?
O1 C1 O1 124.3(7) . 3_656 ?
O1 C1 H1 117.8 . . ?
O1 C1 H1 117.8 3_656 . ?
N1 C4 N2 121.9(12) . 2_575 ?
N1 C4 N2 121.8(12) . . ?
N2 C4 N2 116(2) . 2_575 ?
C4 N1 H1A 132(8) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -171.5(2) . . . 2_575 ?
Er1 O4 C3 O3 -174.0(4) 5_666 . . . ?
Er1 O4 C3 C3 6.1(11) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -156.1(11) . . . 3_656 ?
Er1 O3 C3 O4 -174.0(6) . . . . ?
Er1 O3 C3 C3 6.0(9) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 24_GUA03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_34_gua03
_database_code_depnum_ccdc_archive 'CCDC 2320839'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_34_gua03            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness..
;
_vrf_PLAT088_34_gua03            
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.22 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT242_34_gua03            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C4 Check
RESPONSE: High pressure model approaching upper pressure limit of the crystal.
;
_vrf_PLAT342_34_gua03            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.06 Ang.
RESPONSE: combination of heavy and light elements present in structure. 
;
_vrf_PLAT911_34_gua03            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.449         97 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        34_GUA03
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   7.801(2)
_cell_length_b                   6.5107(13)
_cell_length_c                   19.64(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     997.5(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1842
_cell_measurement_temperature    300
_cell_measurement_theta_max      12.602
_cell_measurement_theta_min      2.139
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.744
_exptl_absorpt_coefficient_mu    3.058
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'Solvothermal synthesis,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.223
_diffrn_reflns_Laue_measured_fraction_max 0.534
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1288
_diffrn_reflns_point_group_measured_fraction_full 0.223
_diffrn_reflns_point_group_measured_fraction_max 0.534
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         12.602
_diffrn_reflns_theta_min         2.139
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.223
_diffrn_measured_fraction_theta_max 0.534
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                102
_reflns_number_total             203
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.772
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         203
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      0.658
_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)+(0.0725P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1038
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Restrained distances
 N1-H1A
 0.9 with sigma of 0.05
 H1A-C4
 2 with sigma of 0.02
3. Restrained planarity
 O4_$1, O3, C3, O4, C3_$1, O3_$1
 with sigma of 0.1
 N2, C4, H2A, H2B, N1, N2_$2, H1A, H1A_$2, H2A_$2, H2B_$2
 with sigma of 0.1
 N1, C4, N2, H1A, H2A, H2B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(O3) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O2) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O1) = Uanis(C1)
Uanis(O3) = Uanis(O4)
Uanis(C3) = Uanis(O3) = Uanis(O4)
Uanis(C2) = Uanis(O2)
5. Rigid body (RIGU) restrains
 O2, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, C3, O4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Er1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
6.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.6174(3) 0.080(2) Uani 1 2 d S TU P . .
O2 O 0.243(3) 0.835(2) 0.653(2) 0.082(12) Uani 1 1 d . U . . .
O4 O 0.507(3) 0.341(5) 0.436(3) 0.125(11) Uani 1 1 d . U . . .
O1 O 0.444(4) 0.495(4) 0.694(4) 0.137(11) Uani 1 1 d . U . . .
O3 O 0.344(3) 0.316(4) 0.524(3) 0.125(11) Uani 1 1 d . U . . .
C2 C 0.2500 1.0000 0.621(4) 0.082(12) Uani 1 2 d S TU P . .
H2 H 0.2500 1.0000 0.5738 0.099 Uiso 1 2 calc R U P . .
C3 C 0.451(4) 0.392(7) 0.489(3) 0.125(11) Uani 1 1 d . U . . .
C1 C 0.5000 0.422(11) 0.7500 0.137(11) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2791 0.7500 0.165 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.340(5) 0.090(18) Uani 1 2 d DS TU P . .
N1 N 0.2500 1.0000 0.405(8) 0.15(2) Uani 1 2 d DS TU P . .
N2 N 0.334(3) 1.138(4) 0.302(4) 0.14(2) Uani 1 1 d . U . . .
H2A H 0.3920 1.2338 0.3207 0.169 Uiso 1 1 calc R U . . .
H2B H 0.3289 1.1300 0.2579 0.169 Uiso 1 1 calc R U . . .
H1A H 0.306(18) 1.09(3) 0.434(8) 0.169 Uiso 1 1 d D U . . .


_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 O2 2.289(19) . ?
Er1 O2 2.289(19) 2_565 ?
Er1 O4 2.40(3) 5_666 ?
Er1 O4 2.40(3) 6_556 ?
Er1 O1 2.14(5) . ?
Er1 O1 2.14(5) 2_565 ?
Er1 O3 2.31(5) 2_565 ?
Er1 O3 2.31(5) . ?
O2 C2 1.25(5) . ?
O4 Er1 2.40(3) 5_666 ?
O4 C3 1.19(8) . ?
O1 C1 1.27(5) . ?
O3 C3 1.18(5) . ?
C2 O2 1.25(5) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.65(11) 5_666 ?
C1 O1 1.27(5) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.28(18) . ?
C4 N2 1.34(7) 2_575 ?
C4 N2 1.34(7) . ?
N1 H1A 0.93(6) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 144(2) . 2_565 ?
O2 Er1 O4 121.8(9) . 6_556 ?
O2 Er1 O4 74.9(11) 2_565 6_556 ?
O2 Er1 O4 121.8(9) 2_565 5_666 ?
O2 Er1 O4 74.9(11) . 5_666 ?
O2 Er1 O3 75.0(13) . 2_565 ?
O2 Er1 O3 138.0(13) 2_565 2_565 ?
O2 Er1 O3 75.0(13) 2_565 . ?
O2 Er1 O3 138.0(13) . . ?
O4 Er1 O4 128(3) 6_556 5_666 ?
O1 Er1 O2 75.8(11) 2_565 . ?
O1 Er1 O2 79.3(13) 2_565 2_565 ?
O1 Er1 O2 75.8(11) . 2_565 ?
O1 Er1 O2 79.3(13) . . ?
O1 Er1 O4 149.4(13) 2_565 5_666 ?
O1 Er1 O4 75.8(19) . 5_666 ?
O1 Er1 O4 75.8(19) 2_565 6_556 ?
O1 Er1 O4 149.4(13) . 6_556 ?
O1 Er1 O1 90(3) 2_565 . ?
O1 Er1 O3 142.4(11) 2_565 . ?
O1 Er1 O3 109.1(18) 2_565 2_565 ?
O1 Er1 O3 142.4(11) . 2_565 ?
O1 Er1 O3 109.1(18) . . ?
O3 Er1 O4 71.3(14) 2_565 5_666 ?
O3 Er1 O4 71.3(14) . 6_556 ?
O3 Er1 O4 68.1(13) . 5_666 ?
O3 Er1 O4 68.1(13) 2_565 6_556 ?
O3 Er1 O3 75(2) 2_565 . ?
C2 O2 Er1 132(4) . . ?
C3 O4 Er1 124(4) . 5_666 ?
C1 O1 Er1 149(3) . . ?
C3 O3 Er1 117(4) . . ?
O2 C2 O2 120(7) 2_575 . ?
O2 C2 H2 120.1 2_575 . ?
O2 C2 H2 120.1 . . ?
O4 C3 C3 107(6) . 5_666 ?
O3 C3 O4 130(7) . . ?
O3 C3 C3 123(7) . 5_666 ?
O1 C1 O1 136(9) . 3_656 ?
O1 C1 H1 112.1 3_656 . ?
O1 C1 H1 112.1 . . ?
N1 C4 N2 124(5) . . ?
N1 C4 N2 124(5) . 2_575 ?
N2 C4 N2 112(9) 2_575 . ?
C4 N1 H1A 128(10) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -175(2) . . . 2_575 ?
Er1 O4 C3 O3 -172(2) 5_666 . . . ?
Er1 O4 C3 C3 9(3) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -130(10) . . . 3_656 ?
Er1 O3 C3 O4 -172(3) . . . . ?
Er1 O3 C3 C3 8(3) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 'in a DAC with PTM of 4:1methanol:ethanol.'
_olex2_submission_original_sample_id 34_GUA03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_11_gua03
_database_code_depnum_ccdc_archive 'CCDC 2320834'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_11_gua03            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.489 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT974_11_gua03            
;
PROBLEM: Check Calcd Negative Resid. Density on       Er1      -2.65 eA-3
RESPONSE: No absorption correction applied, Er is a heavy element.
;
_vrf_PLAT911_11_gua03            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        277 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        11_GUA03
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   8.49580(10)
_cell_length_b                   6.59460(10)
_cell_length_c                   19.201(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1075.78(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2131
_cell_measurement_temperature    300
_cell_measurement_theta_max      26.484
_cell_measurement_theta_min      2.111
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.759
_exptl_absorpt_coefficient_mu    2.835
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'solvothermal synthesis.,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.489
_diffrn_reflns_Laue_measured_fraction_max 0.291
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5278
_diffrn_reflns_point_group_measured_fraction_full 0.489
_diffrn_reflns_point_group_measured_fraction_max 0.291
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         26.484
_diffrn_reflns_theta_min         2.111
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.489
_diffrn_measured_fraction_theta_max 0.291
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                683
_reflns_number_total             1019
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1019
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0197
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0181P)²+2.4466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0591
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-H1A
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O2) = Uanis(C2)
4. Rigid body (RIGU) restrains
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.b X=CH2 refined with riding coordinates:
 N2(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 0.2500 0.5000 0.61610(2) 0.0158(2) Uani 1 2 d S T P . .
O2 O 0.2392(4) 0.8335(4) 0.6574(4) 0.028(2) Uani 1 1 d . . . . .
O4 O 0.5240(4) 0.3326(5) 0.4315(4) 0.037(3) Uani 1 1 d . . . . .
O1 O 0.4322(4) 0.5090(5) 0.7027(5) 0.0407(15) Uani 1 1 d . U . . .
O3 O 0.3556(4) 0.3209(4) 0.5203(4) 0.035(3) Uani 1 1 d . . . . .
C2 C 0.2500 1.0000 0.6265(6) 0.028(2) Uani 1 2 d S T P . .
H2 H 0.2500 1.0000 0.5781 0.034 Uiso 1 2 calc R U P . .
C3 C 0.4665(5) 0.3994(6) 0.4848(6) 0.029(4) Uani 1 1 d . . . . .
C1 C 0.5000 0.4228(9) 0.7500 0.0279(18) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2818 0.7500 0.034 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.3453(13) 0.049(3) Uani 1 2 d S TU P . .
N1 N 0.2500 1.0000 0.4126(16) 0.083(4) Uani 1 2 d DS TU P . .
H1A H 0.320(9) 1.065(13) 0.439(5) 0.100 Uiso 1 1 d D U . . .
N2 N 0.3375(6) 1.1306(7) 0.3091(6) 0.059(5) Uani 1 1 d . . . . .
H2A H 0.3956 1.2172 0.3305 0.070 Uiso 1 1 calc R U . . .
H2B H 0.3359 1.1281 0.2643 0.070 Uiso 1 1 calc R U . . .


_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 O2 2.340(4) . ?
Er1 O2 2.340(4) 2_565 ?
Er1 O4 2.396(4) 6_556 ?
Er1 O4 2.396(4) 5_666 ?
Er1 O1 2.272(6) 2_565 ?
Er1 O1 2.272(6) . ?
Er1 O3 2.363(6) . ?
Er1 O3 2.363(6) 2_565 ?
O2 C2 1.252(7) . ?
O4 Er1 2.396(4) 5_666 ?
O4 C3 1.218(11) . ?
O1 C1 1.217(7) . ?
O3 C3 1.272(8) . ?
C2 O2 1.252(7) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.557(11) 5_666 ?
C1 O1 1.217(7) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.29(4) . ?
C4 N2 1.333(15) . ?
C4 N2 1.333(15) 2_575 ?
N1 H1A 0.89(2) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 140.3(3) . 2_565 ?
O2 Er1 O4 122.06(13) 2_565 5_666 ?
O2 Er1 O4 122.06(13) . 6_556 ?
O2 Er1 O4 74.21(15) . 5_666 ?
O2 Er1 O4 74.21(15) 2_565 6_556 ?
O2 Er1 O3 138.47(18) . . ?
O2 Er1 O3 77.3(2) . 2_565 ?
O2 Er1 O3 138.47(18) 2_565 2_565 ?
O2 Er1 O3 77.3(2) 2_565 . ?
O4 Er1 O4 135.2(4) 6_556 5_666 ?
O1 Er1 O2 75.76(17) 2_565 2_565 ?
O1 Er1 O2 75.76(16) . . ?
O1 Er1 O2 75.50(16) 2_565 . ?
O1 Er1 O2 75.50(16) . 2_565 ?
O1 Er1 O4 73.8(2) . 5_666 ?
O1 Er1 O4 146.8(2) . 6_556 ?
O1 Er1 O4 146.8(2) 2_565 5_666 ?
O1 Er1 O4 73.8(2) 2_565 6_556 ?
O1 Er1 O1 85.9(4) . 2_565 ?
O1 Er1 O3 108.9(2) 2_565 2_565 ?
O1 Er1 O3 144.61(13) 2_565 . ?
O1 Er1 O3 144.61(13) . 2_565 ?
O1 Er1 O3 108.9(2) . . ?
O3 Er1 O4 77.13(18) . 6_556 ?
O3 Er1 O4 68.23(15) . 5_666 ?
O3 Er1 O4 77.13(18) 2_565 5_666 ?
O3 Er1 O4 68.23(15) 2_565 6_556 ?
O3 Er1 O3 77.7(3) . 2_565 ?
C2 O2 Er1 131.3(7) . . ?
C3 O4 Er1 118.4(3) . 5_666 ?
C1 O1 Er1 149.0(3) . . ?
C3 O3 Er1 119.6(4) . . ?
O2 C2 O2 123.3(11) 2_575 . ?
O2 C2 H2 118.3 2_575 . ?
O2 C2 H2 118.3 . . ?
O4 C3 O3 126.9(5) . . ?
O4 C3 C3 118.4(7) . 5_666 ?
O3 C3 C3 114.7(9) . 5_666 ?
O1 C1 O1 124.3(7) 3_656 . ?
O1 C1 H1 117.8 3_656 . ?
O1 C1 H1 117.8 . . ?
N1 C4 N2 121.4(10) . 2_575 ?
N1 C4 N2 121.4(10) . . ?
N2 C4 N2 117(2) . 2_575 ?
C4 N1 H1A 124(9) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -171.0(3) . . . 2_575 ?
Er1 O4 C3 O3 -173.7(5) 5_666 . . . ?
Er1 O4 C3 C3 5.6(12) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -159.2(11) . . . 3_656 ?
Er1 O3 C3 O4 -174.0(7) . . . . ?
Er1 O3 C3 C3 6.6(10) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 'in a diamond anvil cell.'
_olex2_submission_original_sample_id 11_GUA03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_36_gua03
_database_code_depnum_ccdc_archive 'CCDC 2320836'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_36_gua03            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_36_gua03            
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.24 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT342_36_gua03            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.07 Ang.
RESPONSE: A combination of heavy and light elements present.
;
_vrf_PLAT911_36_gua03            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.553        112 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        36_GUA03
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   7.736(8)
_cell_length_b                   6.479(5)
_cell_length_c                   19.71(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     988(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1994
_cell_measurement_temperature    300
_cell_measurement_theta_max      15.601
_cell_measurement_theta_min      2.149
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.742
_exptl_absorpt_coefficient_mu    3.087
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.726
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'Solvothermal synthesis,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.441
_diffrn_reflns_Laue_measured_fraction_max 0.556
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2407
_diffrn_reflns_point_group_measured_fraction_full 0.441
_diffrn_reflns_point_group_measured_fraction_max 0.556
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         15.601
_diffrn_reflns_theta_min         2.149
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.441
_diffrn_measured_fraction_theta_max 0.556
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                223
_reflns_number_total             393
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.457
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.350
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         393
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.1159
_refine_ls_restrained_S_all      1.016
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2877
_refine_ls_wR_factor_ref         0.3100
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Restrained distances
 N1-H1A
 0.9 with sigma of 0.05
 H1A-C4
 2 with sigma of 0.2
 N1-C4 \\sim C4-N2
 with sigma of 0.02
3. Restrained planarity
 O4_$1, O3, C3, O4, C3_$1, O3_$1
 with sigma of 0.1
 C4, N1, N2, N2_$2, H1A, H1A_$2, H2A, H2B, H2A_$2, H2B_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(O3) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O2) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O1) = Uanis(C1)
Uanis(O3) = Uanis(O4)
Uanis(C3) = Uanis(O3) = Uanis(O4)
Uanis(C2) = Uanis(O2)
5. Rigid body (RIGU) restrains
 O2, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, C3, O4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
6.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.6173(2) 0.080(3) Uani 1 2 d S T P . .
O2 O 0.253(2) 0.832(4) 0.653(3) 0.098(12) Uani 1 1 d . U . . .
O4 O 0.504(4) 0.349(4) 0.435(3) 0.125(10) Uani 1 1 d . U . . .
O1 O 0.458(6) 0.494(3) 0.700(5) 0.137(16) Uani 1 1 d . U . . .
O3 O 0.351(3) 0.310(4) 0.525(2) 0.125(10) Uani 1 1 d . U . . .
C2 C 0.2500 1.0000 0.626(5) 0.098(12) Uani 1 2 d S TU P . .
H2 H 0.2500 1.0000 0.5788 0.117 Uiso 1 2 calc R U P . .
C3 C 0.451(4) 0.387(8) 0.487(3) 0.125(10) Uani 1 1 d . U . . .
C1 C 0.5000 0.403(11) 0.7500 0.137(16) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2596 0.7500 0.165 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.329(4) 0.111(18) Uani 1 2 d DS TU P . .
N1 N 0.2500 1.0000 0.393(5) 0.12(2) Uani 1 2 d DS TU P . .
N2 N 0.337(4) 1.147(4) 0.304(3) 0.128(18) Uani 1 1 d D U . . .
H2A H 0.3884 1.2326 0.3309 0.153 Uiso 1 1 calc R U . . .
H2B H 0.3458 1.1609 0.2611 0.153 Uiso 1 1 calc R U . . .
H1A H 0.30(2) 1.08(4) 0.423(13) 0.153 Uiso 1 1 d D U . . .


_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 O2 2.26(3) 2_565 ?
Er1 O2 2.26(3) . ?
Er1 O4 2.37(3) 6_556 ?
Er1 O4 2.37(3) 5_666 ?
Er1 O1 2.30(7) . ?
Er1 O1 2.30(7) 2_565 ?
Er1 O3 2.33(4) 2_565 ?
Er1 O3 2.33(4) . ?
O2 C2 1.21(5) . ?
O4 Er1 2.37(3) 5_666 ?
O4 C3 1.15(7) . ?
O1 C1 1.19(7) . ?
O3 C3 1.18(6) . ?
C2 O2 1.21(5) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.73(12) 5_666 ?
C1 O1 1.19(7) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.26(4) . ?
C4 N2 1.26(4) 2_575 ?
C4 N2 1.26(4) . ?
N1 H1A 0.90(5) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 144(3) 2_565 . ?
O2 Er1 O4 122.2(10) . 6_556 ?
O2 Er1 O4 122.2(10) 2_565 5_666 ?
O2 Er1 O4 74.4(13) . 5_666 ?
O2 Er1 O4 74.4(13) 2_565 6_556 ?
O2 Er1 O1 77.8(13) . . ?
O2 Er1 O1 76.9(12) . 2_565 ?
O2 Er1 O1 77.8(13) 2_565 2_565 ?
O2 Er1 O1 76.9(12) 2_565 . ?
O2 Er1 O3 75.0(16) . 2_565 ?
O2 Er1 O3 137.5(14) 2_565 2_565 ?
O2 Er1 O3 75.0(16) 2_565 . ?
O2 Er1 O3 137.5(14) . . ?
O4 Er1 O4 129(3) 5_666 6_556 ?
O1 Er1 O4 76(2) 2_565 6_556 ?
O1 Er1 O4 149.7(17) . 6_556 ?
O1 Er1 O4 76(2) . 5_666 ?
O1 Er1 O4 149.7(17) 2_565 5_666 ?
O1 Er1 O1 89(4) . 2_565 ?
O1 Er1 O3 143.1(12) 2_565 . ?
O1 Er1 O3 143.1(12) . 2_565 ?
O1 Er1 O3 108.4(19) 2_565 2_565 ?
O1 Er1 O3 108.4(19) . . ?
O3 Er1 O4 73.3(14) . 6_556 ?
O3 Er1 O4 67.2(12) 2_565 6_556 ?
O3 Er1 O4 67.2(12) . 5_666 ?
O3 Er1 O4 73.3(14) 2_565 5_666 ?
O3 Er1 O3 77.1(19) 2_565 . ?
C2 O2 Er1 136(4) . . ?
C3 O4 Er1 126(4) . 5_666 ?
C1 O1 Er1 142(3) . . ?
C3 O3 Er1 119(4) . . ?
O2 C2 O2 129(7) 2_575 . ?
O2 C2 H2 115.7 2_575 . ?
O2 C2 H2 115.7 . . ?
O4 C3 O3 136(7) . . ?
O4 C3 C3 106(5) . 5_666 ?
O3 C3 C3 118(7) . 5_666 ?
O1 C1 O1 120(9) 3_656 . ?
O1 C1 H1 119.9 . . ?
O1 C1 H1 119.9 3_656 . ?
N1 C4 N2 112(4) . . ?
N1 C4 N2 112(4) . 2_575 ?
N2 C4 N2 135(8) 2_575 . ?
C4 N1 H1A 132(10) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 177(2) . . . 2_575 ?
Er1 O4 C3 O3 -166(2) 5_666 . . . ?
Er1 O4 C3 C3 14(3) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -134(9) . . . 3_656 ?
Er1 O3 C3 O4 -167(3) . . . . ?
Er1 O3 C3 C3 13(3) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 36_GUA03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_22_gua03
_database_code_depnum_ccdc_archive 'CCDC 2320837'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_22_gua03            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.471 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT974_22_gua03            
;
PROBLEM: Check Calcd Negative Resid. Density on       Er1      -2.27 eA-3
RESPONSE: No absorption correction applied, Er is a heavy element.
;
_vrf_PLAT911_22_gua03            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        290 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:16 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        22_GUA04
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   8.41540(18)
_cell_length_b                   6.57240(8)
_cell_length_c                   19.210(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1062.49(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2931
_cell_measurement_temperature    300
_cell_measurement_theta_max      26.065
_cell_measurement_theta_min      2.118
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.756
_exptl_absorpt_coefficient_mu    2.871
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_preparation       
'Solvothermal synthesis,Magnetic properties,Negative Linear Compressibility'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.011
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.471
_diffrn_reflns_Laue_measured_fraction_max 0.296
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5174
_diffrn_reflns_point_group_measured_fraction_full 0.471
_diffrn_reflns_point_group_measured_fraction_max 0.296
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         26.065
_diffrn_reflns_theta_min         2.118
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.471
_diffrn_measured_fraction_theta_max 0.296
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                633
_reflns_number_total             976
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         976
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0197
_refine_ls_restrained_S_all      1.039
_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)+(0.0281P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0562
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-H1A
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) = Uanis(C2)
4. Rigid body (RIGU) restrains
 C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.2500 0.5000 0.61609(2) 0.0179(2) Uani 1 2 d S T P . .
O2 O 0.2390(2) 0.8333(3) 0.6581(3) 0.0315(19) Uani 1 1 d . . . . .
O4 O 0.5231(3) 0.3328(3) 0.4309(3) 0.046(3) Uani 1 1 d . . . . .
O1 O 0.4336(3) 0.5076(3) 0.7018(4) 0.050(2) Uani 1 1 d . U . . .
O3 O 0.3553(2) 0.3195(3) 0.5201(3) 0.037(2) Uani 1 1 d . . . . .
C2 C 0.2500 1.0000 0.6279(4) 0.0315(19) Uani 1 2 d S T P . .
H2 H 0.2500 1.0000 0.5794 0.038 Uiso 1 2 calc R U P . .
C3 C 0.4657(4) 0.3989(5) 0.4857(4) 0.035(4) Uani 1 1 d . . . . .
C1 C 0.5000 0.4212(7) 0.7500 0.035(2) Uani 1 2 d S TU P . .
H1 H 0.5000 0.2797 0.7500 0.042 Uiso 1 2 calc R U P . .
C4 C 0.2500 1.0000 0.3429(14) 0.060(4) Uani 1 2 d S TU P . .
N1 N 0.2500 1.0000 0.4129(16) 0.101(6) Uani 1 2 d DS TU P . .
H1A H 0.293(8) 1.088(11) 0.443(4) 0.121 Uiso 1 1 d D U . . .
N2 N 0.3369(4) 1.1307(4) 0.3091(4) 0.064(4) Uani 1 1 d . . . . .
H2A H 0.3370 1.1308 0.2643 0.076 Uiso 1 1 calc R U . . .
H2B H 0.3943 1.2169 0.3315 0.076 Uiso 1 1 calc R U . . .


_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 O2 2.337(3) 2_565 ?
Er1 O2 2.337(3) . ?
Er1 O4 2.381(3) 5_666 ?
Er1 O4 2.381(3) 6_556 ?
Er1 O1 2.259(6) 2_565 ?
Er1 O1 2.259(6) . ?
Er1 O3 2.364(4) 2_565 ?
Er1 O3 2.364(4) . ?
O2 C2 1.244(5) . ?
O4 Er1 2.381(3) 5_666 ?
O4 C3 1.237(9) . ?
O1 C1 1.221(6) . ?
O3 C3 1.255(6) . ?
C2 O2 1.244(5) 2_575 ?
C2 H2 0.9300 . ?
C3 C3 1.550(9) 5_666 ?
C1 O1 1.221(6) 3_656 ?
C1 H1 0.9300 . ?
C4 N1 1.34(4) . ?
C4 N2 1.302(14) 2_575 ?
C4 N2 1.302(14) . ?
N1 H1A 0.89(2) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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 Er1 O2 139.6(3) 2_565 . ?
O2 Er1 O4 122.14(9) 2_565 5_666 ?
O2 Er1 O4 74.34(12) . 5_666 ?
O2 Er1 O4 122.14(9) . 6_556 ?
O2 Er1 O4 74.34(12) 2_565 6_556 ?
O2 Er1 O3 139.01(14) 2_565 2_565 ?
O2 Er1 O3 77.54(16) . 2_565 ?
O2 Er1 O3 139.01(14) . . ?
O2 Er1 O3 77.54(16) 2_565 . ?
O4 Er1 O4 135.5(3) 6_556 5_666 ?
O1 Er1 O2 75.79(12) 2_565 2_565 ?
O1 Er1 O2 75.02(12) 2_565 . ?
O1 Er1 O2 75.79(12) . . ?
O1 Er1 O2 75.02(12) . 2_565 ?
O1 Er1 O4 73.6(2) . 5_666 ?
O1 Er1 O4 146.63(15) 2_565 5_666 ?
O1 Er1 O4 146.63(15) . 6_556 ?
O1 Er1 O4 73.6(2) 2_565 6_556 ?
O1 Er1 O1 86.4(3) . 2_565 ?
O1 Er1 O3 144.46(10) . 2_565 ?
O1 Er1 O3 108.86(17) . . ?
O1 Er1 O3 144.46(10) 2_565 . ?
O1 Er1 O3 108.86(17) 2_565 2_565 ?
O3 Er1 O4 76.90(14) . 6_556 ?
O3 Er1 O4 68.63(12) 2_565 6_556 ?
O3 Er1 O4 68.63(12) . 5_666 ?
O3 Er1 O4 76.90(14) 2_565 5_666 ?
O3 Er1 O3 77.54(18) 2_565 . ?
C2 O2 Er1 131.4(5) . . ?
C3 O4 Er1 118.3(2) . 5_666 ?
C1 O1 Er1 148.8(2) . . ?
C3 O3 Er1 118.7(3) . . ?
O2 C2 O2 124.2(8) 2_575 . ?
O2 C2 H2 117.9 2_575 . ?
O2 C2 H2 117.9 . . ?
O4 C3 O3 126.3(4) . . ?
O4 C3 C3 117.3(6) . 5_666 ?
O3 C3 C3 116.4(8) . 5_666 ?
O1 C1 O1 124.6(5) 3_656 . ?
O1 C1 H1 117.7 . . ?
O1 C1 H1 117.7 3_656 . ?
N2 C4 N1 119.9(11) . . ?
N2 C4 N1 119.9(11) 2_575 . ?
N2 C4 N2 120(2) . 2_575 ?
C4 N1 H1A 131(7) . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

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 O2 C2 O2 -170.89(19) . . . 2_575 ?
Er1 O4 C3 O3 -173.8(4) 5_666 . . . ?
Er1 O4 C3 C3 7.2(9) 5_666 . . 5_666 ?
Er1 O1 C1 O1 -156.2(9) . . . 3_656 ?
Er1 O3 C3 O4 -173.0(5) . . . . ?
Er1 O3 C3 C3 5.9(8) . . . 5_666 ?

_olex2_exptl_crystal_mounting_method 
'in a diamond anvil cell, with PTM of 4:1 Methanol:Ethanol.'
_olex2_submission_original_sample_id 22_GUA03
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_16_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320852'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_16_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.327 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_16_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.48 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT242_16_dma01            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Er1 Check
RESPONSE: no absorption correction applied, Er is a heavy element.
;
_vrf_PLAT342_16_dma01            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.
RESPONSE: A combination of heavy and light elements is present in the structure, and only a single C-C bond is present.
;
_vrf_PLAT911_16_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        510 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-12-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        16_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   9.1183(8)
_cell_length_b                   8.948(5)
_cell_length_c                   13.1042(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.446(5)
_cell_angle_gamma                90
_cell_volume                     1062.5(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1780
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      20.311
_cell_measurement_theta_min      1.771
_shelx_estimated_absorpt_T_max   0.700
_shelx_estimated_absorpt_T_min   0.531
_exptl_absorpt_coefficient_mu    2.867
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.447
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_preparation       'solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.327
_diffrn_reflns_Laue_measured_fraction_max 0.295
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4752
_diffrn_reflns_point_group_measured_fraction_full 0.327
_diffrn_reflns_point_group_measured_fraction_max 0.295
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         20.311
_diffrn_reflns_theta_min         1.771
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.327
_diffrn_measured_fraction_theta_max 0.295
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                555
_reflns_number_total             959
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         959
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0519
_refine_ls_restrained_S_all      0.846
_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)+(0.1298P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1664
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 O3, C3, C4, O4, O6, O5
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C5 \\sim N1 \\sim C6: within 2A with sigma of 0.05 and sigma for terminal atoms
of 0.1 within 2A
O5 \\sim O6 \\sim C4 \\sim C3 \\sim O4 \\sim O3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1 \\sim C1 \\sim O8: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C6, N1, C5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C2, O7, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C4, O4, C3, O3, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_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 0.2500 0.2837(2) 0.7500 0.0440(13) Uani 1 2 d S T P . .
Er2 Er 0.7500 0.74217(19) 0.7500 0.0447(15) Uani 1 2 d S T P . .
O4 O 0.3456(13) 0.481(4) 0.6589(8) 0.083(11) Uani 1 1 d . U . . .
O3 O 0.4665(15) 0.374(5) 0.8411(10) 0.095(11) Uani 1 1 d . U . . .
O6 O 0.5300(15) 0.668(4) 0.6612(9) 0.080(11) Uani 1 1 d . U . . .
C3 C 0.5335(19) 0.488(4) 0.8006(11) 0.072(11) Uani 1 1 d . U . . .
O1 O 0.0721(19) 0.094(6) 0.7338(11) 0.12(2) Uani 1 1 d . U . . .
C4 C 0.4599(17) 0.548(4) 0.6988(11) 0.062(11) Uani 1 1 d . U . . .
C2 C 0.2695(19) 0.255(5) 0.5049(9) 0.110(15) Uani 1 1 d . U . . .
H2 H 0.2862 0.3571 0.5023 0.132 Uiso 1 1 calc R U . . .
O2 O 0.256(2) 0.177(4) 0.4207(8) 0.112(13) Uani 1 1 d . U . . .
O7 O 0.261(2) 0.195(4) 0.5863(8) 0.121(14) Uani 1 1 d . U . . .
C6 C 0.338(4) -0.222(7) 0.432(3) 0.132(13) Uani 1 1 d . U . . .
H6A H 0.4069 -0.1541 0.4070 0.197 Uiso 1 1 calc R U . . .
H6B H 0.3224 -0.3055 0.3860 0.197 Uiso 1 1 calc R U . . .
H6C H 0.3769 -0.2576 0.4989 0.197 Uiso 1 1 calc R U . . .
O5 O 0.6507(14) 0.544(4) 0.8396(9) 0.091(12) Uani 1 1 d . U . . .
C1 C 0.020(2) -0.011(7) 0.7624(13) 0.11(2) Uani 1 1 d . U . . .
H1 H 0.0848 -0.0686 0.8058 0.130 Uiso 1 1 calc R U . . .
O8 O -0.0894(17) -0.057(5) 0.7497(11) 0.12(2) Uani 1 1 d . U . . .
N1 N 0.188(2) -0.140(6) 0.4396(12) 0.160(10) Uani 1 1 d . U . . .
H1A H 0.1989 -0.0328 0.4342 0.192 Uiso 1 1 calc R U . . .
H1B H 0.1126 -0.1741 0.3864 0.192 Uiso 1 1 calc R U . . .
C5 C 0.150(4) -0.186(6) 0.5475(18) 0.111(11) Uani 1 1 d . U . . .
H5A H 0.1307 -0.2910 0.5488 0.167 Uiso 1 1 calc R U . . .
H5B H 0.0638 -0.1319 0.5629 0.167 Uiso 1 1 calc R U . . .
H5C H 0.2314 -0.1618 0.5978 0.167 Uiso 1 1 calc R U . . .


_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 O4 2.35(2) . ?
Er1 O4 2.35(2) 2_556 ?
Er1 O3 2.334(19) . ?
Er1 O3 2.334(19) 2_556 ?
Er1 O1 2.34(4) . ?
Er1 O1 2.34(4) 2_556 ?
Er1 O7 2.300(14) . ?
Er1 O7 2.299(14) 2_556 ?
Er2 O6 2.300(17) . ?
Er2 O6 2.300(17) 2_656 ?
Er2 O2 2.344(13) 4_666 ?
Er2 O2 2.344(13) 3_666 ?
Er2 O5 2.37(3) 2_656 ?
Er2 O5 2.37(3) . ?
Er2 O8 2.32(3) 2_566 ?
Er2 O8 2.32(3) 1_665 ?
O4 C4 1.27(3) . ?
O3 C3 1.33(4) . ?
O6 C4 1.37(4) . ?
C3 C4 1.52(3) . ?
C3 O5 1.24(3) . ?
O1 C1 1.14(6) . ?
C2 H2 0.9300 . ?
C2 O2 1.30(3) . ?
C2 O7 1.20(2) . ?
O2 Er2 2.344(13) 3_666 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 N1 1.57(6) . ?
C1 H1 0.9300 . ?
C1 O8 1.07(3) . ?
O8 Er2 2.32(3) 1_445 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
N1 C5 1.55(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
O4 Er1 O4 82.9(12) 2_556 . ?
O3 Er1 O4 70.1(8) 2_556 2_556 ?
O3 Er1 O4 79.7(9) 2_556 . ?
O3 Er1 O4 70.1(8) . . ?
O3 Er1 O4 79.7(9) . 2_556 ?
O3 Er1 O3 139(2) 2_556 . ?
O3 Er1 O1 70.6(15) 2_556 . ?
O3 Er1 O1 70.6(15) . 2_556 ?
O3 Er1 O1 146.7(11) 2_556 2_556 ?
O3 Er1 O1 146.7(11) . . ?
O1 Er1 O4 107.3(11) . 2_556 ?
O1 Er1 O4 107.3(11) 2_556 . ?
O1 Er1 O4 142.2(6) 2_556 2_556 ?
O1 Er1 O4 142.2(6) . . ?
O1 Er1 O1 87(2) . 2_556 ?
O7 Er1 O4 142.1(8) 2_556 . ?
O7 Er1 O4 74.1(9) . . ?
O7 Er1 O4 142.1(8) . 2_556 ?
O7 Er1 O4 74.1(9) 2_556 2_556 ?
O7 Er1 O3 118.3(7) 2_556 2_556 ?
O7 Er1 O3 76.4(8) 2_556 . ?
O7 Er1 O3 118.3(7) . . ?
O7 Er1 O3 76.4(8) . 2_556 ?
O7 Er1 O1 74.5(8) 2_556 . ?
O7 Er1 O1 76.6(8) 2_556 2_556 ?
O7 Er1 O1 74.5(8) . 2_556 ?
O7 Er1 O1 76.6(8) . . ?
O7 Er1 O7 139.8(15) 2_556 . ?
O6 Er2 O6 146.7(19) . 2_656 ?
O6 Er2 O2 71.4(7) 2_656 4_666 ?
O6 Er2 O2 119.7(6) . 4_666 ?
O6 Er2 O2 119.7(6) 2_656 3_666 ?
O6 Er2 O2 71.4(7) . 3_666 ?
O6 Er2 O5 83.9(8) . 2_656 ?
O6 Er2 O5 71.0(8) 2_656 2_656 ?
O6 Er2 O5 71.0(8) . . ?
O6 Er2 O5 83.9(8) 2_656 . ?
O6 Er2 O8 73.0(12) 2_656 1_665 ?
O6 Er2 O8 73.0(12) . 2_566 ?
O6 Er2 O8 137.5(10) 2_656 2_566 ?
O6 Er2 O8 137.5(10) . 1_665 ?
O2 Er2 O2 144.3(17) 4_666 3_666 ?
O2 Er2 O5 137.4(8) 3_666 . ?
O2 Er2 O5 74.1(10) 4_666 . ?
O2 Er2 O5 137.4(8) 4_666 2_656 ?
O2 Er2 O5 74.1(10) 3_666 2_656 ?
O5 Er2 O5 82.6(13) 2_656 . ?
O8 Er2 O2 79.5(9) 2_566 3_666 ?
O8 Er2 O2 79.5(9) 1_665 4_666 ?
O8 Er2 O2 72.9(8) 1_665 3_666 ?
O8 Er2 O2 72.9(8) 2_566 4_666 ?
O8 Er2 O5 107.7(10) 1_665 2_656 ?
O8 Er2 O5 149.3(6) 2_566 2_656 ?
O8 Er2 O5 149.3(6) 1_665 . ?
O8 Er2 O5 107.7(10) 2_566 . ?
O8 Er2 O8 78.5(18) 1_665 2_566 ?
C4 O4 Er1 118.9(14) . . ?
C3 O3 Er1 117.5(12) . . ?
C4 O6 Er2 117.3(12) . . ?
O3 C3 C4 116(2) . . ?
O5 C3 O3 123.9(19) . . ?
O5 C3 C4 120(3) . . ?
C1 O1 Er1 151.9(18) . . ?
O4 C4 O6 128.4(17) . . ?
O4 C4 C3 117(3) . . ?
O6 C4 C3 114(2) . . ?
O2 C2 H2 119.7 . . ?
O7 C2 H2 119.7 . . ?
O7 C2 O2 121(3) . . ?
C2 O2 Er2 130(2) . 3_666 ?
C2 O7 Er1 134(2) . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
C3 O5 Er2 117.2(16) . . ?
O1 C1 H1 113.3 . . ?
O8 C1 O1 133(5) . . ?
O8 C1 H1 113.3 . . ?
C1 O8 Er2 151(5) . 1_445 ?
C6 N1 H1A 111.2 . . ?
C6 N1 H1B 111.2 . . ?
H1A N1 H1B 109.1 . . ?
C5 N1 C6 103(3) . . ?
C5 N1 H1A 111.2 . . ?
C5 N1 H1B 111.2 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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 C4 O6 -177.2(19) . . . . ?
Er1 O4 C4 C3 4(2) . . . . ?
Er1 O3 C3 C4 0(2) . . . . ?
Er1 O3 C3 O5 -178(2) . . . . ?
Er1 O1 C1 O8 155(6) . . . . ?
Er2 O6 C4 O4 -173.7(19) . . . . ?
Er2 O6 C4 C3 5(2) . . . . ?
O3 C3 C4 O4 -3(2) . . . . ?
O3 C3 C4 O6 178.1(17) . . . . ?
O3 C3 O5 Er2 178.5(17) . . . . ?
O1 C1 O8 Er2 159(5) . . . 1_445 ?
C4 C3 O5 Er2 0(2) . . . . ?
O2 C2 O7 Er1 -171.4(19) . . . . ?
O7 C2 O2 Er2 175.4(18) . . . 3_666 ?
O5 C3 C4 O4 175(2) . . . . ?
O5 C3 C4 O6 -4(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 MeOH:EtOH'
_olex2_submission_original_sample_id 16_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_14_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320851'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_14_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.318 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_14_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.94 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT242_14_dma01            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Er1 Check
RESPONSE: no absorption correction applied, Er is a heavy element.
;
_vrf_PLAT911_14_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        528 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-12-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        14_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   9.1326(5)
_cell_length_b                   8.974(4)
_cell_length_c                   13.1405(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.410(4)
_cell_angle_gamma                90
_cell_volume                     1070.2(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2045
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      21.251
_cell_measurement_theta_min      1.768
_shelx_estimated_absorpt_T_max   0.702
_shelx_estimated_absorpt_T_min   0.533
_exptl_absorpt_coefficient_mu    2.846
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_preparation       'solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.318
_diffrn_reflns_Laue_measured_fraction_max 0.275
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5013
_diffrn_reflns_point_group_measured_fraction_full 0.318
_diffrn_reflns_point_group_measured_fraction_max 0.275
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         21.251
_diffrn_reflns_theta_min         1.768
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.318
_diffrn_measured_fraction_theta_max 0.275
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                623
_reflns_number_total             1027
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1027
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0450
_refine_ls_restrained_S_all      0.957
_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)+(0.1046P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1563
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 O3, C3, C4, O4, O6, O5
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C5 \\sim N1 \\sim C6: within 2A with sigma of 0.05 and sigma for terminal atoms
of 0.1 within 2A
O5 \\sim O6 \\sim C4 \\sim C3 \\sim O4 \\sim O3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1 \\sim C1 \\sim O8: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C6, N1, C5
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
 C2, O7, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C4, O4, C3, O3, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_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 0.2500 0.2842(2) 0.7500 0.0384(12) Uani 1 2 d S T P . .
Er2 Er 0.7500 0.74225(17) 0.7500 0.0387(13) Uani 1 2 d S T P . .
O4 O 0.3453(12) 0.487(3) 0.6608(7) 0.082(11) Uani 1 1 d . U . . .
O3 O 0.4671(13) 0.373(4) 0.8402(9) 0.087(10) Uani 1 1 d . U . . .
O6 O 0.5287(14) 0.666(4) 0.6614(8) 0.075(10) Uani 1 1 d . U . . .
C3 C 0.5342(16) 0.489(3) 0.7996(10) 0.066(10) Uani 1 1 d . U . . .
O1 O 0.0741(18) 0.088(5) 0.7330(9) 0.111(18) Uani 1 1 d . U . . .
C4 C 0.4629(16) 0.552(4) 0.7002(11) 0.058(10) Uani 1 1 d . U . . .
C2 C 0.2680(14) 0.249(3) 0.5026(7) 0.077(12) Uani 1 1 d . U . . .
H2 H 0.2847 0.3507 0.5001 0.093 Uiso 1 1 calc R U . . .
O2 O 0.2576(17) 0.180(3) 0.4201(7) 0.085(11) Uani 1 1 d . U . . .
O7 O 0.2585(18) 0.195(3) 0.5858(7) 0.094(12) Uani 1 1 d . U . . .
C6 C 0.329(2) -0.224(5) 0.441(2) 0.127(17) Uani 1 1 d . U . . .
H6A H 0.3993 -0.1550 0.4186 0.190 Uiso 1 1 calc R U . . .
H6B H 0.3203 -0.3086 0.3966 0.190 Uiso 1 1 calc R U . . .
H6C H 0.3618 -0.2554 0.5098 0.190 Uiso 1 1 calc R U . . .
O5 O 0.6515(13) 0.541(4) 0.8377(8) 0.087(11) Uani 1 1 d . U . . .
C1 C 0.026(2) -0.014(6) 0.7665(13) 0.090(18) Uani 1 1 d . U . . .
H1 H 0.0869 -0.0678 0.8144 0.108 Uiso 1 1 calc R U . . .
O8 O -0.0898(15) -0.056(4) 0.7473(9) 0.095(18) Uani 1 1 d . U . . .
N1 N 0.185(2) -0.150(6) 0.4394(12) 0.147(10) Uani 1 1 d . U . . .
H1A H 0.1931 -0.0429 0.4306 0.176 Uiso 1 1 calc R U . . .
H1B H 0.1142 -0.1899 0.3860 0.176 Uiso 1 1 calc R U . . .
C5 C 0.147(3) -0.188(5) 0.5407(16) 0.099(14) Uani 1 1 d . U . . .
H5A H 0.1438 -0.2941 0.5476 0.149 Uiso 1 1 calc R U . . .
H5B H 0.0528 -0.1462 0.5499 0.149 Uiso 1 1 calc R U . . .
H5C H 0.2204 -0.1478 0.5916 0.149 Uiso 1 1 calc R U . . .


_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 O4 2.38(2) 2_556 ?
Er1 O4 2.38(2) . ?
Er1 O3 2.335(16) . ?
Er1 O3 2.335(16) 2_556 ?
Er1 O1 2.38(3) 2_556 ?
Er1 O1 2.38(3) . ?
Er1 O7 2.312(13) . ?
Er1 O7 2.312(13) 2_556 ?
Er2 O6 2.322(15) 2_656 ?
Er2 O6 2.322(15) . ?
Er2 O2 2.334(12) 4_666 ?
Er2 O2 2.334(12) 3_666 ?
Er2 O5 2.37(2) 2_656 ?
Er2 O5 2.37(2) . ?
Er2 O8 2.33(3) 2_566 ?
Er2 O8 2.33(3) 1_665 ?
O4 C4 1.28(3) . ?
O3 C3 1.34(3) . ?
O6 C4 1.31(4) . ?
C3 C4 1.51(3) . ?
C3 O5 1.23(2) . ?
O1 C1 1.13(5) . ?
C2 H2 0.9300 . ?
C2 O2 1.24(2) . ?
C2 O7 1.207(19) . ?
O2 Er2 2.334(12) 3_666 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 N1 1.47(4) . ?
C1 H1 0.9300 . ?
C1 O8 1.12(3) . ?
O8 Er2 2.33(3) 1_445 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
N1 C5 1.45(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
O4 Er1 O4 80.2(11) . 2_556 ?
O3 Er1 O4 79.9(8) 2_556 . ?
O3 Er1 O4 69.6(7) 2_556 2_556 ?
O3 Er1 O4 79.9(8) . 2_556 ?
O3 Er1 O4 69.6(7) . . ?
O3 Er1 O3 139.8(18) 2_556 . ?
O3 Er1 O1 146.0(9) 2_556 2_556 ?
O3 Er1 O1 146.0(9) . . ?
O3 Er1 O1 71.3(12) 2_556 . ?
O3 Er1 O1 71.3(12) . 2_556 ?
O1 Er1 O4 109.4(9) 2_556 . ?
O1 Er1 O4 109.4(9) . 2_556 ?
O1 Er1 O4 143.1(5) . . ?
O1 Er1 O4 143.1(5) 2_556 2_556 ?
O1 Er1 O1 84.4(17) 2_556 . ?
O7 Er1 O4 75.8(8) 2_556 2_556 ?
O7 Er1 O4 141.0(7) . 2_556 ?
O7 Er1 O4 75.8(8) . . ?
O7 Er1 O4 141.0(7) 2_556 . ?
O7 Er1 O3 118.5(6) 2_556 2_556 ?
O7 Er1 O3 76.2(7) 2_556 . ?
O7 Er1 O3 118.5(6) . . ?
O7 Er1 O3 76.2(7) . 2_556 ?
O7 Er1 O1 75.4(7) 2_556 2_556 ?
O7 Er1 O1 74.8(7) 2_556 . ?
O7 Er1 O1 75.4(7) . . ?
O7 Er1 O1 74.8(6) . 2_556 ?
O7 Er1 O7 139.4(13) 2_556 . ?
O6 Er2 O6 145.5(17) 2_656 . ?
O6 Er2 O2 120.0(5) . 4_666 ?
O6 Er2 O2 71.2(6) 2_656 4_666 ?
O6 Er2 O2 71.2(6) . 3_666 ?
O6 Er2 O2 120.0(5) 2_656 3_666 ?
O6 Er2 O5 70.2(7) 2_656 2_656 ?
O6 Er2 O5 83.5(8) . 2_656 ?
O6 Er2 O5 83.5(8) 2_656 . ?
O6 Er2 O5 70.2(7) . . ?
O6 Er2 O8 137.3(8) . 1_665 ?
O6 Er2 O8 137.3(8) 2_656 2_566 ?
O6 Er2 O8 74.1(11) . 2_566 ?
O6 Er2 O8 74.1(11) 2_656 1_665 ?
O2 Er2 O2 145.3(14) 4_666 3_666 ?
O2 Er2 O5 136.1(7) 3_666 . ?
O2 Er2 O5 74.6(9) 4_666 . ?
O2 Er2 O5 136.1(7) 4_666 2_656 ?
O2 Er2 O5 74.6(8) 3_666 2_656 ?
O5 Er2 O5 81.0(12) 2_656 . ?
O8 Er2 O2 80.3(7) 2_566 3_666 ?
O8 Er2 O2 80.3(7) 1_665 4_666 ?
O8 Er2 O2 72.8(7) 1_665 3_666 ?
O8 Er2 O2 72.8(7) 2_566 4_666 ?
O8 Er2 O5 108.1(8) 1_665 2_656 ?
O8 Er2 O5 150.6(5) 2_566 2_656 ?
O8 Er2 O5 150.6(5) 1_665 . ?
O8 Er2 O5 108.1(8) 2_566 . ?
O8 Er2 O8 78.0(14) 1_665 2_566 ?
C4 O4 Er1 119.0(14) . . ?
C3 O3 Er1 117.5(11) . . ?
C4 O6 Er2 116.4(11) . . ?
O3 C3 C4 117.7(18) . . ?
O5 C3 O3 123.5(18) . . ?
O5 C3 C4 119(3) . . ?
C1 O1 Er1 148.8(16) . . ?
O4 C4 O6 126.5(16) . . ?
O4 C4 C3 116(2) . . ?
O6 C4 C3 117.4(18) . . ?
O2 C2 H2 117.0 . . ?
O7 C2 H2 117.0 . . ?
O7 C2 O2 126(3) . . ?
C2 O2 Er2 133(2) . 3_666 ?
C2 O7 Er1 136(2) . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
C3 O5 Er2 117.1(16) . . ?
O1 C1 H1 117.1 . . ?
O8 C1 O1 126(4) . . ?
O8 C1 H1 117.1 . . ?
C1 O8 Er2 146(4) . 1_445 ?
C6 N1 H1A 111.7 . . ?
C6 N1 H1B 111.7 . . ?
H1A N1 H1B 109.4 . . ?
C5 N1 C6 101(3) . . ?
C5 N1 H1A 111.7 . . ?
C5 N1 H1B 111.7 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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 C4 O6 -179.6(19) . . . . ?
Er1 O4 C4 C3 2(2) . . . . ?
Er1 O3 C3 C4 1(2) . . . . ?
Er1 O3 C3 O5 -177.1(18) . . . . ?
Er1 O1 C1 O8 154(4) . . . . ?
Er2 O6 C4 O4 -175.7(18) . . . . ?
Er2 O6 C4 C3 2(2) . . . . ?
O3 C3 C4 O4 -2(2) . . . . ?
O3 C3 C4 O6 179.5(18) . . . . ?
O3 C3 O5 Er2 179.0(16) . . . . ?
O1 C1 O8 Er2 161(4) . . . 1_445 ?
C4 C3 O5 Er2 1(2) . . . . ?
O2 C2 O7 Er1 -173.0(17) . . . . ?
O7 C2 O2 Er2 173.5(16) . . . 3_666 ?
O5 C3 C4 O4 176(2) . . . . ?
O5 C3 C4 O6 -2(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 MeOH:EtOH'
_olex2_submission_original_sample_id 14_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_12_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320846'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_12_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.316 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_12_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.86 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT241_12_dma01            
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
RESPONSE: no absorption correction applied, Er is a heavy element.
;
_vrf_PLAT242_12_dma01            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Er1 Check
RESPONSE: no absorption correction applied, Er is a heavy element.
;
_vrf_PLAT911_12_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        531 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-12-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        12_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   9.1263(6)
_cell_length_b                   8.963(4)
_cell_length_c                   13.1305(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.440(4)
_cell_angle_gamma                90
_cell_volume                     1067.3(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2382
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      21.226
_cell_measurement_theta_min      1.769
_shelx_estimated_absorpt_T_max   0.701
_shelx_estimated_absorpt_T_min   0.532
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.436
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_preparation       'solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.316
_diffrn_reflns_Laue_measured_fraction_max 0.274
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4991
_diffrn_reflns_point_group_measured_fraction_full 0.316
_diffrn_reflns_point_group_measured_fraction_max 0.274
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         21.226
_diffrn_reflns_theta_min         1.769
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.316
_diffrn_measured_fraction_theta_max 0.274
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                633
_reflns_number_total             1016
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1016
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0409
_refine_ls_restrained_S_all      0.988
_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)+(0.0921P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1458
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 O3, C3, C4, O4, O6, O5
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C5 \\sim N1 \\sim C6: within 2A with sigma of 0.05 and sigma for terminal atoms
of 0.1 within 2A
O5 \\sim O6 \\sim C4 \\sim C3 \\sim O4 \\sim O3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1 \\sim C1 \\sim O8: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C6, N1, C5
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
 C2, O7, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C4, O4, C3, O3, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_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 0.2500 0.2848(2) 0.7500 0.0369(11) Uani 1 2 d S T P . .
Er2 Er 0.7500 0.74282(16) 0.7500 0.0367(12) Uani 1 2 d S T P . .
O4 O 0.3466(11) 0.486(3) 0.6614(7) 0.082(10) Uani 1 1 d . U . . .
O3 O 0.4690(12) 0.379(4) 0.8398(8) 0.086(10) Uani 1 1 d . U . . .
O6 O 0.5268(13) 0.663(4) 0.6615(7) 0.076(9) Uani 1 1 d . U . . .
C3 C 0.5351(17) 0.491(3) 0.7997(10) 0.073(10) Uani 1 1 d . U . . .
O1 O 0.0761(17) 0.089(5) 0.7328(8) 0.119(16) Uani 1 1 d . U . . .
C4 C 0.4641(15) 0.552(3) 0.7002(10) 0.061(10) Uani 1 1 d . U . . .
C2 C 0.2692(15) 0.252(3) 0.5019(7) 0.084(11) Uani 1 1 d . U . . .
H2 H 0.2880 0.3543 0.4997 0.101 Uiso 1 1 calc R U . . .
O2 O 0.2584(15) 0.181(3) 0.4205(6) 0.084(10) Uani 1 1 d . U . . .
O7 O 0.2563(16) 0.195(3) 0.5852(6) 0.091(11) Uani 1 1 d . U . . .
C6 C 0.336(3) -0.219(6) 0.440(3) 0.13(2) Uani 1 1 d . U . . .
H6A H 0.4012 -0.1488 0.4133 0.198 Uiso 1 1 calc R U . . .
H6B H 0.3297 -0.3074 0.3982 0.198 Uiso 1 1 calc R U . . .
H6C H 0.3728 -0.2447 0.5089 0.198 Uiso 1 1 calc R U . . .
O5 O 0.6510(12) 0.543(3) 0.8376(7) 0.087(11) Uani 1 1 d . U . . .
C1 C 0.0262(18) -0.010(5) 0.7662(11) 0.090(15) Uani 1 1 d . U . . .
H1 H 0.0870 -0.0619 0.8155 0.108 Uiso 1 1 calc R U . . .
O8 O -0.0924(13) -0.056(4) 0.7471(7) 0.095(16) Uani 1 1 d . U . . .
N1 N 0.187(2) -0.152(5) 0.4384(11) 0.133(14) Uani 1 1 d . U . . .
H1A H 0.1906 -0.0446 0.4282 0.160 Uiso 1 1 calc R U . . .
H1B H 0.1187 -0.1948 0.3843 0.160 Uiso 1 1 calc R U . . .
C5 C 0.142(3) -0.187(5) 0.5395(15) 0.094(18) Uani 1 1 d . U . . .
H5A H 0.1267 -0.2925 0.5446 0.141 Uiso 1 1 calc R U . . .
H5B H 0.0520 -0.1354 0.5482 0.141 Uiso 1 1 calc R U . . .
H5C H 0.2179 -0.1560 0.5918 0.141 Uiso 1 1 calc R U . . .


_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 O4 2.37(2) . ?
Er1 O4 2.37(2) 2_556 ?
Er1 O3 2.360(15) . ?
Er1 O3 2.360(15) 2_556 ?
Er1 O1 2.36(3) 2_556 ?
Er1 O1 2.36(3) . ?
Er1 O7 2.315(12) 2_556 ?
Er1 O7 2.315(12) . ?
Er2 O6 2.339(14) . ?
Er2 O6 2.339(14) 2_656 ?
Er2 O2 2.332(11) 4_666 ?
Er2 O2 2.332(11) 3_666 ?
Er2 O5 2.36(2) 2_656 ?
Er2 O5 2.36(2) . ?
Er2 O8 2.31(3) 1_665 ?
Er2 O8 2.31(3) 2_566 ?
O4 C4 1.28(2) . ?
O3 C3 1.31(3) . ?
O6 C4 1.29(3) . ?
C3 C4 1.49(3) . ?
C3 O5 1.21(2) . ?
O1 C1 1.11(5) . ?
C2 H2 0.9300 . ?
C2 O2 1.24(2) . ?
C2 O7 1.225(19) . ?
O2 Er2 2.332(11) 3_666 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 N1 1.49(4) . ?
C1 H1 0.9300 . ?
C1 O8 1.16(2) . ?
O8 Er2 2.31(3) 1_445 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
N1 C5 1.47(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
O4 Er1 O4 80.8(10) . 2_556 ?
O3 Er1 O4 79.8(7) . 2_556 ?
O3 Er1 O4 68.4(7) 2_556 2_556 ?
O3 Er1 O4 68.4(7) . . ?
O3 Er1 O4 79.8(7) 2_556 . ?
O3 Er1 O3 138.0(16) . 2_556 ?
O1 Er1 O4 109.2(9) 2_556 . ?
O1 Er1 O4 143.3(5) . . ?
O1 Er1 O4 109.2(9) . 2_556 ?
O1 Er1 O4 143.3(5) 2_556 2_556 ?
O1 Er1 O3 146.9(9) 2_556 2_556 ?
O1 Er1 O3 72.2(11) . 2_556 ?
O1 Er1 O3 146.9(9) . . ?
O1 Er1 O3 72.2(11) 2_556 . ?
O1 Er1 O1 84.1(16) 2_556 . ?
O7 Er1 O4 140.6(6) . 2_556 ?
O7 Er1 O4 140.6(6) 2_556 . ?
O7 Er1 O4 75.9(7) . . ?
O7 Er1 O4 75.9(7) 2_556 2_556 ?
O7 Er1 O3 76.4(6) . 2_556 ?
O7 Er1 O3 118.9(5) 2_556 2_556 ?
O7 Er1 O3 76.4(6) 2_556 . ?
O7 Er1 O3 118.9(5) . . ?
O7 Er1 O1 74.9(6) 2_556 2_556 ?
O7 Er1 O1 75.2(6) 2_556 . ?
O7 Er1 O1 74.9(6) . . ?
O7 Er1 O1 75.2(6) . 2_556 ?
O7 Er1 O7 139.4(12) 2_556 . ?
O6 Er2 O6 144.6(16) 2_656 . ?
O6 Er2 O5 83.5(7) . 2_656 ?
O6 Er2 O5 69.6(6) 2_656 2_656 ?
O6 Er2 O5 69.6(6) . . ?
O6 Er2 O5 83.5(7) 2_656 . ?
O2 Er2 O6 119.9(5) 3_666 2_656 ?
O2 Er2 O6 119.9(5) 4_666 . ?
O2 Er2 O6 71.3(6) 3_666 . ?
O2 Er2 O6 71.3(6) 4_666 2_656 ?
O2 Er2 O2 146.1(13) 4_666 3_666 ?
O2 Er2 O5 74.1(8) 3_666 2_656 ?
O2 Er2 O5 135.7(6) 4_666 2_656 ?
O2 Er2 O5 74.1(8) 4_666 . ?
O2 Er2 O5 135.7(7) 3_666 . ?
O5 Er2 O5 81.4(11) . 2_656 ?
O8 Er2 O6 137.6(8) 2_566 2_656 ?
O8 Er2 O6 74.7(10) 1_665 2_656 ?
O8 Er2 O6 137.6(8) 1_665 . ?
O8 Er2 O6 74.7(10) 2_566 . ?
O8 Er2 O2 73.2(6) 2_566 4_666 ?
O8 Er2 O2 73.2(6) 1_665 3_666 ?
O8 Er2 O2 80.5(6) 2_566 3_666 ?
O8 Er2 O2 80.5(6) 1_665 4_666 ?
O8 Er2 O5 150.8(4) 1_665 . ?
O8 Er2 O5 108.1(8) 2_566 . ?
O8 Er2 O5 108.1(8) 1_665 2_656 ?
O8 Er2 O5 150.8(4) 2_566 2_656 ?
O8 Er2 O8 77.3(13) 1_665 2_566 ?
C4 O4 Er1 119.8(13) . . ?
C3 O3 Er1 118.4(10) . . ?
C4 O6 Er2 116.3(10) . . ?
O3 C3 C4 117.0(17) . . ?
O5 C3 O3 123.4(17) . . ?
O5 C3 C4 120(2) . . ?
C1 O1 Er1 149.1(15) . . ?
O4 C4 O6 126.3(16) . . ?
O4 C4 C3 116(2) . . ?
O6 C4 C3 117.3(18) . . ?
O2 C2 H2 118.4 . . ?
O7 C2 H2 118.4 . . ?
O7 C2 O2 123(3) . . ?
C2 O2 Er2 132.0(19) . 3_666 ?
C2 O7 Er1 134.7(19) . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
C3 O5 Er2 117.1(15) . . ?
O1 C1 H1 116.0 . . ?
O1 C1 O8 128(3) . . ?
O8 C1 H1 116.0 . . ?
C1 O8 Er2 148(3) . 1_445 ?
C6 N1 H1A 110.9 . . ?
C6 N1 H1B 110.9 . . ?
H1A N1 H1B 108.9 . . ?
C5 N1 C6 104(3) . . ?
C5 N1 H1A 110.9 . . ?
C5 N1 H1B 110.9 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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 C4 O6 -178.7(19) . . . . ?
Er1 O4 C4 C3 2(2) . . . . ?
Er1 O3 C3 C4 1(2) . . . . ?
Er1 O3 C3 O5 -176.7(18) . . . . ?
Er1 O1 C1 O8 153(4) . . . . ?
Er2 O6 C4 O4 -176.0(18) . . . . ?
Er2 O6 C4 C3 4(2) . . . . ?
O3 C3 C4 O4 -2(2) . . . . ?
O3 C3 C4 O6 178.7(18) . . . . ?
O3 C3 O5 Er2 179.2(16) . . . . ?
O1 C1 O8 Er2 159(3) . . . 1_445 ?
C4 C3 O5 Er2 2(2) . . . . ?
O2 C2 O7 Er1 -174.4(15) . . . . ?
O7 C2 O2 Er2 172.0(14) . . . 3_666 ?
O5 C3 C4 O4 176(2) . . . . ?
O5 C3 C4 O6 -4(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'in DAc with PTM of 4:1 MeOH:EtOH'
_olex2_submission_original_sample_id 12_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_22_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320848'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_22_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.319 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_22_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.90 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT722_22_dma01            
;
PROBLEM: Angle   Calc      135.00, Rep     131(10) Dev...       4.00 Degree
RESPONSE: High pressure model approaching upper pressure limit of the crystal.
;
_vrf_PLAT234_22_dma01            
;
PROBLEM: Large Hirshfeld Difference Er1      --O1       .       0.30 Ang.
RESPONSE: High pressure model approaching upper pressure limit of the crystal.
;
_vrf_PLAT241_22_dma01            
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
RESPONSE: No absorption correction applied, Er is a heavy element.
;
_vrf_PLAT242_22_dma01            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Er1 Check
RESPONSE: No absorption correction applied, Er is a heavy element.
;
_vrf_PLAT342_22_dma01            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.06 Ang.
RESPONSE: A combination of heavy and light elements is present in the structure, and only a single C-C bond is present.
;
_vrf_PLAT911_22_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        144 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-07-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        22_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/a 1'
_space_group_name_Hall           '-P 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'-x, -y, -z'
'x-1/2, -y, z'

_cell_length_a                   9.0759(5)
_cell_length_b                   8.863(6)
_cell_length_c                   6.4822(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.228(5)
_cell_angle_gamma                90
_cell_volume                     518.3(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1812
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      19.200
_cell_measurement_theta_min      2.161
_shelx_estimated_absorpt_T_max   0.694
_shelx_estimated_absorpt_T_min   0.524
_exptl_absorpt_coefficient_mu    2.938
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.508
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             370
_exptl_crystal_preparation       'Solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.319
_diffrn_reflns_Laue_measured_fraction_max 0.297
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2052
_diffrn_reflns_point_group_measured_fraction_full 0.319
_diffrn_reflns_point_group_measured_fraction_max 0.297
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         19.200
_diffrn_reflns_theta_min         2.161
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.319
_diffrn_measured_fraction_theta_max 0.297
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                345
_reflns_number_total             401
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         401
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0567
_refine_ls_restrained_S_all      1.048
_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)+(0.1043P)²+1.5924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1769
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C1
 1.3 with sigma of 0.1
 C1_$3-C1
 1 with sigma of 0.02
 C4-N1
 1.4 with sigma of 0.02
 O1-C1 \\sim O1-C1_$3
 with sigma of 0.01
3. Restrained planarity
 O3, O4_$1, O4, O3_$1
 with sigma of 0.1
 O4, C3, C3_$2, O3, O4_$2, O3_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O4 \\sim C3 \\sim C3 \\sim O3 \\sim O4 \\sim O3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N1 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O2 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O1) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4) = Uanis(O3) = Uanis(C3) = Uanis(C3) = Uanis(O4) = Uanis(O3)
5. Rigid body (RIGU) restrains
 C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O4, O4, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C4, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C3, O3, O3, C3, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C1(0.5) H1(0.5)
7.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_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 0.7500 -0.7697(3) 0.5000 0.083(2) Uani 1 2 d S T P . .
O1 O 0.575(4) -0.606(12) 0.486(5) 0.194(17) Uani 1 1 d D U . . .
O2 O 0.750(3) -0.676(7) 0.166(3) 0.16(2) Uani 1 1 d . U . . .
O4 O 0.542(3) -0.844(8) 0.312(4) 0.151(13) Uani 1 1 d . U . . .
O3 O 0.645(2) -0.981(7) 0.679(4) 0.151(13) Uani 1 1 d . . . . .
C2 C 0.7500 -0.712(11) 0.0000 0.15(3) Uani 1 2 d S TU P . .
H2 H 0.7500 -0.8171 0.0000 0.178 Uiso 1 2 calc R U P . .
C4 C 0.355(11) -0.77(2) -0.117(17) 0.28(5) Uani 1 1 d D U . . .
H4A H 0.3212 -0.6699 -0.1648 0.420 Uiso 1 1 calc R U . . .
H4B H 0.3673 -0.8308 -0.2348 0.420 Uiso 1 1 calc R U . . .
H4C H 0.4481 -0.7583 -0.0329 0.420 Uiso 1 1 calc R U . . .
N1 N 0.2500 -0.83(3) 0.0000 0.29(5) Uani 1 2 d DS TU P . .
H1A H 0.1923 -0.8993 -0.0968 0.349 Uiso 0.5 1 calc R U P . .
H1B H 0.3077 -0.8993 0.0968 0.349 Uiso 0.5 1 calc R U P . .
C3 C 0.472(3) -0.960(6) 0.396(6) 0.151(13) Uani 1 1 d . U . . .
C1 C 0.544(3) -0.467(3) 0.501(17) 0.19(2) Uani 0.5 1 d D U P . .
H1 H 0.6271 -0.4043 0.5039 0.223 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.14(7) . ?
Er1 O1 2.14(7) 2_656 ?
Er1 O2 2.32(3) . ?
Er1 O2 2.32(3) 2_656 ?
Er1 O4 2.24(3) 2_656 ?
Er1 O4 2.24(3) . ?
Er1 O3 2.45(5) . ?
Er1 O3 2.45(5) 2_656 ?
O1 C1 1.27(7) 3_646 ?
O1 C1 1.27(7) . ?
O2 C2 1.12(3) . ?
O4 C3 1.36(6) . ?
O3 C3 1.23(5) 3_636 ?
C2 O2 1.12(3) 2_655 ?
C2 H2 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 N1 1.41(2) . ?
N1 C4 1.41(2) 2 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
C3 O3 1.23(5) 3_636 ?
C3 C3 1.56(9) 3_636 ?
C1 O1 1.27(7) 3_646 ?
C1 H1 0.9300 . ?

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 Er1 O1 95(5) . 2_656 ?
O1 Er1 O2 73.8(14) 2_656 . ?
O1 Er1 O2 73.8(14) . 2_656 ?
O1 Er1 O2 78.1(14) . . ?
O1 Er1 O2 78.1(14) 2_656 2_656 ?
O1 Er1 O4 143.1(19) . 2_656 ?
O1 Er1 O4 66(3) . . ?
O1 Er1 O4 66(3) 2_656 2_656 ?
O1 Er1 O4 143.1(19) 2_656 . ?
O1 Er1 O3 102(2) 2_656 2_656 ?
O1 Er1 O3 145.2(15) 2_656 . ?
O1 Er1 O3 145.2(15) . 2_656 ?
O1 Er1 O3 102(2) . . ?
O2 Er1 O2 138(3) . 2_656 ?
O2 Er1 O3 77.9(17) 2_656 . ?
O2 Er1 O3 139.2(13) . . ?
O2 Er1 O3 77.9(17) . 2_656 ?
O2 Er1 O3 139.2(13) 2_656 2_656 ?
O4 Er1 O2 121.9(11) 2_656 . ?
O4 Er1 O2 71.5(14) 2_656 2_656 ?
O4 Er1 O2 71.5(14) . . ?
O4 Er1 O2 121.9(11) . 2_656 ?
O4 Er1 O4 146(4) 2_656 . ?
O4 Er1 O3 71.6(15) . . ?
O4 Er1 O3 82.3(15) 2_656 . ?
O4 Er1 O3 71.6(15) 2_656 2_656 ?
O4 Er1 O3 82.3(15) . 2_656 ?
O3 Er1 O3 80(2) . 2_656 ?
C1 O1 Er1 145(5) . . ?
C1 O1 Er1 166(6) 3_646 . ?
C1 O1 C1 46(3) 3_646 . ?
C2 O2 Er1 142(5) . . ?
C3 O4 Er1 114(2) . . ?
C3 O3 Er1 120(3) 3_636 . ?
O2 C2 O2 147(9) 2_655 . ?
O2 C2 H2 106.6 . . ?
O2 C2 H2 106.6 2_655 . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
C4 N1 C4 131(10) 2 . ?
C4 N1 H1A 104.4 . . ?
C4 N1 H1A 104.4 2 . ?
C4 N1 H1B 104.4 . . ?
C4 N1 H1B 104.4 2 . ?
H1A N1 H1B 105.6 . . ?
O4 C3 C3 124(4) . 3_636 ?
O3 C3 O4 126(4) 3_636 . ?
O3 C3 C3 110(6) 3_636 3_636 ?
O1 C1 O1 134(3) 3_646 . ?
O1 C1 H1 113.1 3_646 . ?
O1 C1 H1 113.1 . . ?

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
Er1 O1 C1 O1 -169(5) . . . 3_646 ?
Er1 O2 C2 O2 180(3) . . . 2_655 ?
Er1 O4 C3 O3 180(3) . . . 3_636 ?
Er1 O4 C3 C3 -1(3) . . . 3_636 ?
C1 O1 C1 O1 0.000(1) 3_646 . . 3_646 ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 methanol:ethanol'
_olex2_submission_original_sample_id 22_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320845'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_20_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.315 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_20_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.84 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT234_20_dma01            
;
PROBLEM: Large Hirshfeld Difference Er1      --O1       .       0.28 Ang.
RESPONSE: High pressure model approaching upper pressure limit of the crystal.
;
_vrf_PLAT241_20_dma01            
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
RESPONSE: High pressure model approaching upper pressure limit of the crystal.
;
_vrf_PLAT242_20_dma01            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Er1 Check
RESPONSE: No absorption correction applied, Er is a heavy element.
;
_vrf_PLAT342_20_dma01            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.05 Ang.
RESPONSE: A combination of heavy and light elements is present in the structure, and only a single C-C bond is present.
;
_vrf_PLAT911_20_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        148 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-07-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        20_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/a 1'
_space_group_name_Hall           '-P 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'-x, -y, -z'
'x-1/2, -y, z'

_cell_length_a                   9.0907(8)
_cell_length_b                   8.903(6)
_cell_length_c                   6.5091(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.380(6)
_cell_angle_gamma                90
_cell_volume                     523.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1779
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      19.218
_cell_measurement_theta_min      2.152
_shelx_estimated_absorpt_T_max   0.697
_shelx_estimated_absorpt_T_min   0.527
_exptl_absorpt_coefficient_mu    2.908
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             370
_exptl_crystal_preparation       'Solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.315
_diffrn_reflns_Laue_measured_fraction_max 0.291
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2082
_diffrn_reflns_point_group_measured_fraction_full 0.315
_diffrn_reflns_point_group_measured_fraction_max 0.291
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         19.218
_diffrn_reflns_theta_min         2.152
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.315
_diffrn_measured_fraction_theta_max 0.291
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                319
_reflns_number_total             397
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         397
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      1.093
_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)+(0.0949P)²+1.3693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1615
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C1
 1.3 with sigma of 0.1
 C1_$3-C1
 1 with sigma of 0.02
 C4-N1
 1.4 with sigma of 0.02
 O1-C1 \\sim O1-C1_$3
 with sigma of 0.01
3. Restrained planarity
 O3, O4_$1, O4, O3_$1
 with sigma of 0.1
 O4, C3, C3_$2, O3, O4_$2, O3_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O4 \\sim C3 \\sim C3 \\sim O3 \\sim O4 \\sim O3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N1 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O2 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O1) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4) = Uanis(O3) = Uanis(C3) = Uanis(C3) = Uanis(O4) = Uanis(O3)
5. Rigid body (RIGU) restrains
 C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O4, O4, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C4, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C3, O3, O3, C3, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C1(0.5) H1(0.5)
7.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_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 0.7500 -0.7698(3) 0.5000 0.069(2) Uani 1 2 d S T P . .
O1 O 0.572(4) -0.613(11) 0.485(5) 0.183(16) Uani 1 1 d D U . . .
O2 O 0.752(3) -0.674(7) 0.167(3) 0.16(2) Uani 1 1 d . U . . .
O4 O 0.539(3) -0.852(7) 0.316(4) 0.142(12) Uani 1 1 d . U . . .
O3 O 0.646(2) -0.980(7) 0.682(3) 0.142(12) Uani 1 1 d . . . . .
C2 C 0.7500 -0.715(11) 0.0000 0.16(3) Uani 1 2 d S TU P . .
H2 H 0.7500 -0.8191 0.0000 0.187 Uiso 1 2 calc R U P . .
C4 C 0.360(8) -0.740(16) -0.110(12) 0.20(3) Uani 1 1 d D U . . .
H4A H 0.4429 -0.7107 -0.0146 0.306 Uiso 1 1 calc R U . . .
H4B H 0.3198 -0.6531 -0.1839 0.306 Uiso 1 1 calc R U . . .
H4C H 0.3906 -0.8119 -0.2059 0.306 Uiso 1 1 calc R U . . .
N1 N 0.2500 -0.804(18) 0.0000 0.24(4) Uani 1 2 d DS TU P . .
H1A H 0.1952 -0.8702 -0.0996 0.287 Uiso 0.5 1 calc R U P . .
H1B H 0.3048 -0.8702 0.0996 0.287 Uiso 0.5 1 calc R U P . .
C3 C 0.465(3) -0.971(6) 0.403(5) 0.142(12) Uani 1 1 d . U . . .
C1 C 0.546(2) -0.469(3) 0.504(18) 0.18(2) Uani 0.5 1 d D U P . .
H1 H 0.6320 -0.4116 0.5100 0.217 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.13(6) . ?
Er1 O1 2.13(6) 2_656 ?
Er1 O2 2.33(3) 2_656 ?
Er1 O2 2.33(3) . ?
Er1 O4 2.27(3) 2_656 ?
Er1 O4 2.27(3) . ?
Er1 O3 2.46(5) 2_656 ?
Er1 O3 2.46(5) . ?
O1 C1 1.31(7) . ?
O1 C1 1.31(7) 3_646 ?
O2 C2 1.14(3) . ?
O4 C3 1.41(6) . ?
O3 C3 1.18(4) 3_636 ?
C2 O2 1.14(4) 2_655 ?
C2 H2 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 N1 1.41(2) . ?
N1 C4 1.41(2) 2 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
C3 O3 1.18(4) 3_636 ?
C3 C3 1.45(8) 3_636 ?
C1 O1 1.31(7) 3_646 ?
C1 H1 0.9300 . ?

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 Er1 O1 98(5) . 2_656 ?
O1 Er1 O2 73.6(13) 2_656 . ?
O1 Er1 O2 73.6(13) . 2_656 ?
O1 Er1 O2 78.6(14) . . ?
O1 Er1 O2 78.6(14) 2_656 2_656 ?
O1 Er1 O4 146.0(19) . 2_656 ?
O1 Er1 O4 66(2) . . ?
O1 Er1 O4 66(2) 2_656 2_656 ?
O1 Er1 O4 146.0(19) 2_656 . ?
O1 Er1 O3 143.9(15) 2_656 . ?
O1 Er1 O3 143.9(15) . 2_656 ?
O1 Er1 O3 101(2) 2_656 2_656 ?
O1 Er1 O3 101(2) . . ?
O2 Er1 O2 137(3) 2_656 . ?
O2 Er1 O3 77.6(16) . 2_656 ?
O2 Er1 O3 140.3(13) 2_656 2_656 ?
O2 Er1 O3 77.6(16) 2_656 . ?
O2 Er1 O3 140.3(13) . . ?
O4 Er1 O2 73.8(13) 2_656 2_656 ?
O4 Er1 O2 121.0(10) . 2_656 ?
O4 Er1 O2 73.8(13) . . ?
O4 Er1 O2 121.0(10) 2_656 . ?
O4 Er1 O4 142(3) 2_656 . ?
O4 Er1 O3 70.1(14) 2_656 2_656 ?
O4 Er1 O3 81.3(13) . 2_656 ?
O4 Er1 O3 70.1(14) . . ?
O4 Er1 O3 81.3(13) 2_656 . ?
O3 Er1 O3 81(2) 2_656 . ?
C1 O1 Er1 171(6) 3_646 . ?
C1 O1 Er1 141(4) . . ?
C1 O1 C1 45(3) . 3_646 ?
C2 O2 Er1 140(5) . . ?
C3 O4 Er1 117(2) . . ?
C3 O3 Er1 114(3) 3_636 . ?
O2 C2 O2 143(9) . 2_655 ?
O2 C2 H2 108.4 2_655 . ?
O2 C2 H2 108.4 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
C4 N1 C4 132(10) 2 . ?
C4 N1 H1A 104.2 . . ?
C4 N1 H1A 104.2 2 . ?
C4 N1 H1B 104.2 . . ?
C4 N1 H1B 104.2 2 . ?
H1A N1 H1B 105.5 . . ?
O4 C3 C3 116(5) . 3_636 ?
O3 C3 O4 121(4) 3_636 . ?
O3 C3 C3 124(7) 3_636 3_636 ?
O1 C1 O1 135(3) . 3_646 ?
O1 C1 H1 112.5 . . ?
O1 C1 H1 112.5 3_646 . ?

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 O1 C1 O1 -170(6) . . . 3_646 ?
Er1 O2 C2 O2 178(3) . . . 2_655 ?
Er1 O4 C3 O3 180(3) . . . 3_636 ?
Er1 O4 C3 C3 -1(3) . . . 3_636 ?
C1 O1 C1 O1 0.000(3) 3_646 . . 3_646 ?

_olex2_exptl_crystal_mounting_method 
'in a diamond anvil cell with pressure transmitting media of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 20_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_08_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320849'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_08_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.316 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_08_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.97 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT911_08_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        532 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-12-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        08_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   9.1539(3)
_cell_length_b                   8.9987(19)
_cell_length_c                   13.1797(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.604(2)
_cell_angle_gamma                90
_cell_volume                     1078.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2978
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      25.626
_cell_measurement_theta_min      1.761
_shelx_estimated_absorpt_T_max   0.703
_shelx_estimated_absorpt_T_min   0.535
_exptl_absorpt_coefficient_mu    2.824
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_preparation       'solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.316
_diffrn_reflns_Laue_measured_fraction_max 0.185
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5341
_diffrn_reflns_point_group_measured_fraction_full 0.316
_diffrn_reflns_point_group_measured_fraction_max 0.185
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         25.626
_diffrn_reflns_theta_min         1.761
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.316
_diffrn_measured_fraction_theta_max 0.185
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                882
_reflns_number_total             1180
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1180
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0414
_refine_ls_restrained_S_all      1.039
_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)+(0.1065P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1461
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 O3, C3, C4, O4, O6, O5
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
O5 \\sim O6 \\sim C4 \\sim C3 \\sim O4 \\sim O3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C2, O7, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C4, O4, C3, O3, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, N1, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_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 0.2500 0.28635(16) 0.7500 0.0304(8) Uani 1 2 d S T P . .
Er2 Er 0.7500 0.74417(13) 0.7500 0.0309(8) Uani 1 2 d S T P . .
O4 O 0.3466(7) 0.485(2) 0.6618(4) 0.062(7) Uani 1 1 d . U . . .
O3 O 0.4689(9) 0.374(3) 0.8405(5) 0.080(7) Uani 1 1 d . U . . .
O6 O 0.5269(9) 0.662(3) 0.6623(5) 0.069(7) Uani 1 1 d . U . . .
C3 C 0.5337(10) 0.484(2) 0.8015(6) 0.063(7) Uani 1 1 d . U . . .
O1 O 0.0747(12) 0.098(3) 0.7326(6) 0.096(10) Uani 1 1 d . U . . .
C4 C 0.4610(10) 0.549(3) 0.6988(6) 0.054(7) Uani 1 1 d . U . . .
C2 C 0.2706(10) 0.244(3) 0.5018(4) 0.071(8) Uani 1 1 d . U . . .
H2 H 0.2916 0.3451 0.4990 0.086 Uiso 1 1 calc R U . . .
O2 O 0.2573(12) 0.173(2) 0.4200(5) 0.069(8) Uani 1 1 d . U . . .
O7 O 0.2578(13) 0.190(2) 0.5859(5) 0.077(9) Uani 1 1 d . U . . .
C6 C 0.326(2) -0.236(5) 0.4268(18) 0.133(18) Uani 1 1 d . U . . .
H6A H 0.3992 -0.1639 0.4154 0.200 Uiso 1 1 calc R U . . .
H6B H 0.3128 -0.3038 0.3702 0.200 Uiso 1 1 calc R U . . .
H6C H 0.3561 -0.2902 0.4884 0.200 Uiso 1 1 calc R U . . .
O5 O 0.6519(7) 0.545(2) 0.8381(4) 0.076(8) Uani 1 1 d . U . . .
C1 C 0.0263(12) -0.012(4) 0.7666(7) 0.075(10) Uani 1 1 d . U . . .
H1 H 0.0885 -0.0658 0.8138 0.090 Uiso 1 1 calc R U . . .
O8 O -0.0908(9) -0.057(3) 0.7457(6) 0.077(10) Uani 1 1 d . U . . .
N1 N 0.1810(10) -0.158(3) 0.4369(6) 0.099(15) Uani 1 1 d . U . . .
H1A H 0.1929 -0.0515 0.4282 0.119 Uiso 1 1 calc R U . . .
H1B H 0.1063 -0.1924 0.3840 0.119 Uiso 1 1 calc R U . . .
C5 C 0.134(2) -0.188(4) 0.5381(10) 0.091(17) Uani 1 1 d . U . . .
H5A H 0.0532 -0.2562 0.5311 0.137 Uiso 1 1 calc R U . . .
H5B H 0.1045 -0.0968 0.5675 0.137 Uiso 1 1 calc R U . . .
H5C H 0.2147 -0.2305 0.5817 0.137 Uiso 1 1 calc R U . . .


_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 O4 2.360(14) . ?
Er1 O4 2.360(14) 2_556 ?
Er1 O3 2.349(11) 2_556 ?
Er1 O3 2.349(11) . ?
Er1 O1 2.33(2) . ?
Er1 O1 2.33(2) 2_556 ?
Er1 O7 2.340(10) 2_556 ?
Er1 O7 2.340(10) . ?
Er2 O6 2.347(10) 2_656 ?
Er2 O6 2.347(10) . ?
Er2 O2 2.354(9) 3_666 ?
Er2 O2 2.354(9) 4_666 ?
Er2 O5 2.368(16) . ?
Er2 O5 2.368(16) 2_656 ?
Er2 O8 2.31(2) 2_566 ?
Er2 O8 2.31(2) 1_665 ?
O4 C4 1.245(16) . ?
O3 C3 1.29(2) . ?
O6 C4 1.30(3) . ?
C3 C4 1.554(18) . ?
C3 O5 1.257(16) . ?
O1 C1 1.19(4) . ?
C2 H2 0.9300 . ?
C2 O2 1.246(16) . ?
C2 O7 1.231(14) . ?
O2 Er2 2.354(9) 3_666 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 N1 1.52(3) . ?
C1 H1 0.9300 . ?
C1 O8 1.149(17) . ?
O8 Er2 2.31(2) 1_445 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
N1 C5 1.473(18) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
O4 Er1 O4 81.4(7) . 2_556 ?
O3 Er1 O4 80.8(6) . 2_556 ?
O3 Er1 O4 69.4(5) . . ?
O3 Er1 O4 69.4(5) 2_556 2_556 ?
O3 Er1 O4 80.8(6) 2_556 . ?
O3 Er1 O3 140.6(13) . 2_556 ?
O1 Er1 O4 107.9(6) . 2_556 ?
O1 Er1 O4 107.9(6) 2_556 . ?
O1 Er1 O4 142.8(3) . . ?
O1 Er1 O4 142.8(3) 2_556 2_556 ?
O1 Er1 O3 69.9(9) . 2_556 ?
O1 Er1 O3 69.9(9) 2_556 . ?
O1 Er1 O3 146.5(6) 2_556 2_556 ?
O1 Er1 O3 146.5(6) . . ?
O1 Er1 O1 86.6(12) 2_556 . ?
O1 Er1 O7 74.5(5) . . ?
O1 Er1 O7 74.1(5) 2_556 . ?
O1 Er1 O7 74.1(5) . 2_556 ?
O1 Er1 O7 74.5(5) 2_556 2_556 ?
O7 Er1 O4 76.9(6) . . ?
O7 Er1 O4 76.9(6) 2_556 2_556 ?
O7 Er1 O4 142.2(5) . 2_556 ?
O7 Er1 O4 142.2(5) 2_556 . ?
O7 Er1 O3 118.7(4) 2_556 2_556 ?
O7 Er1 O3 76.8(5) . 2_556 ?
O7 Er1 O3 118.7(4) . . ?
O7 Er1 O3 76.8(5) 2_556 . ?
O7 Er1 O7 136.3(10) 2_556 . ?
O6 Er2 O6 143.4(12) . 2_656 ?
O6 Er2 O2 72.7(4) . 3_666 ?
O6 Er2 O2 119.7(4) . 4_666 ?
O6 Er2 O2 119.7(4) 2_656 3_666 ?
O6 Er2 O2 72.7(4) 2_656 4_666 ?
O6 Er2 O5 69.3(4) . . ?
O6 Er2 O5 83.0(5) 2_656 . ?
O6 Er2 O5 83.0(5) . 2_656 ?
O6 Er2 O5 69.3(4) 2_656 2_656 ?
O2 Er2 O2 143.2(11) 4_666 3_666 ?
O2 Er2 O5 75.1(6) 3_666 2_656 ?
O2 Er2 O5 137.3(5) 3_666 . ?
O2 Er2 O5 137.3(5) 4_666 2_656 ?
O2 Er2 O5 75.1(6) 4_666 . ?
O5 Er2 O5 81.6(8) . 2_656 ?
O8 Er2 O6 75.0(7) 2_566 . ?
O8 Er2 O6 138.2(5) 2_566 2_656 ?
O8 Er2 O6 75.0(7) 1_665 2_656 ?
O8 Er2 O6 138.2(5) 1_665 . ?
O8 Er2 O2 80.2(5) 2_566 3_666 ?
O8 Er2 O2 71.4(5) 1_665 3_666 ?
O8 Er2 O2 71.4(5) 2_566 4_666 ?
O8 Er2 O2 80.2(5) 1_665 4_666 ?
O8 Er2 O5 150.9(3) 1_665 . ?
O8 Er2 O5 150.9(3) 2_566 2_656 ?
O8 Er2 O5 107.4(6) 2_566 . ?
O8 Er2 O5 107.4(6) 1_665 2_656 ?
O8 Er2 O8 78.6(9) 1_665 2_566 ?
C4 O4 Er1 120.3(8) . . ?
C3 O3 Er1 117.5(7) . . ?
C4 O6 Er2 118.5(7) . . ?
O3 C3 C4 117.7(12) . . ?
O5 C3 O3 126.6(10) . . ?
O5 C3 C4 115.7(16) . . ?
C1 O1 Er1 148.1(9) . . ?
O4 C4 O6 128.5(10) . . ?
O4 C4 C3 115.0(17) . . ?
O6 C4 C3 116.5(12) . . ?
O2 C2 H2 117.8 . . ?
O7 C2 H2 117.8 . . ?
O7 C2 O2 124(2) . . ?
C2 O2 Er2 130.6(15) . 3_666 ?
C2 O7 Er1 134.5(16) . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
C3 O5 Er2 120.0(9) . . ?
O1 C1 H1 117.3 . . ?
O8 C1 O1 125(2) . . ?
O8 C1 H1 117.3 . . ?
C1 O8 Er2 147(2) . 1_445 ?
C6 N1 H1A 109.7 . . ?
C6 N1 H1B 109.7 . . ?
H1A N1 H1B 108.2 . . ?
C5 N1 C6 110(2) . . ?
C5 N1 H1A 109.7 . . ?
C5 N1 H1B 109.7 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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 C4 O6 -178.0(14) . . . . ?
Er1 O4 C4 C3 2.3(17) . . . . ?
Er1 O3 C3 C4 0.4(18) . . . . ?
Er1 O3 C3 O5 -179.2(13) . . . . ?
Er1 O1 C1 O8 159(3) . . . . ?
Er2 O6 C4 O4 -176.5(13) . . . . ?
Er2 O6 C4 C3 3.2(19) . . . . ?
O3 C3 C4 O4 -1.8(19) . . . . ?
O3 C3 C4 O6 178.5(11) . . . . ?
O3 C3 O5 Er2 179.2(13) . . . . ?
O1 C1 O8 Er2 165(2) . . . 1_445 ?
C4 C3 O5 Er2 -0.4(17) . . . . ?
O2 C2 O7 Er1 -172.3(12) . . . . ?
O7 C2 O2 Er2 172.2(11) . . . 3_666 ?
O5 C3 C4 O4 177.8(12) . . . . ?
O5 C3 C4 O6 -1.9(19) . . . . ?

_olex2_exptl_crystal_mounting_method 
'in DAC with pressure transmitting media of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 08_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_24_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320847'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_24_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.322 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_24_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.83 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT234_24_dma01            
;
PROBLEM: Large Hirshfeld Difference Er1      --O1       .       0.37 Ang.
RESPONSE: High pressure model approaching upper pressure limit of the crystal.
;
_vrf_PLAT241_24_dma01            
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
RESPONSE: no absorption correction applied, Er is a heavy element.
;
_vrf_PLAT242_24_dma01            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Er1 Check
RESPONSE: no absorption correction applied, Er is a heavy element.
;
_vrf_PLAT342_24_dma01            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.05 Ang.
RESPONSE: A combination of heavy and light elements is present in the structure, and only a single C-C bond is present.
;
_vrf_PLAT911_24_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        144 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-07-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        24_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/a 1'
_space_group_name_Hall           '-P 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'-x, -y, -z'
'x-1/2, -y, z'

_cell_length_a                   9.0471(15)
_cell_length_b                   8.792(11)
_cell_length_c                   6.4339(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.131(10)
_cell_angle_gamma                90
_cell_volume                     508.9(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1626
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      17.138
_cell_measurement_theta_min      2.177
_shelx_estimated_absorpt_T_max   0.690
_shelx_estimated_absorpt_T_min   0.518
_exptl_absorpt_coefficient_mu    2.993
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             370
_exptl_crystal_preparation       'Solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.322
_diffrn_reflns_Laue_measured_fraction_max 0.320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1551
_diffrn_reflns_point_group_measured_fraction_full 0.322
_diffrn_reflns_point_group_measured_fraction_max 0.320
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         17.138
_diffrn_reflns_theta_min         2.177
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.322
_diffrn_measured_fraction_theta_max 0.320
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                236
_reflns_number_total             306
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         306
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      0.991
_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)+(0.1157P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1460
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-N1
 1.4 with sigma of 0.02
 O1-C1
 1.3 with sigma of 0.1
 C1_$3-C1
 1 with sigma of 0.2
 O1_$3-C1 \\sim O1-C1
 with sigma of 0.1
3. Restrained planarity
 O3, O4_$1, O4, O3_$1
 with sigma of 0.1
 O4, C3, C3_$2, O3, O4_$2, O3_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O2 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O1 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C4 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(O1) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 O4, C3, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, N1
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
6. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C1(0.5) H1(0.5)
7.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_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 0.7500 -0.7700(3) 0.5000 0.097(2) Uani 1 2 d S T P . .
O1 O 0.582(5) -0.599(15) 0.484(6) 0.24(2) Uani 1 1 d D U . . .
O2 O 0.745(4) -0.665(8) 0.157(3) 0.20(3) Uani 1 1 d . U . . .
O4 O 0.549(4) -0.866(11) 0.311(5) 0.19(3) Uani 1 1 d . U . . .
O3 O 0.636(3) -0.983(10) 0.687(5) 0.19(4) Uani 1 1 d . U . . .
C2 C 0.7500 -0.705(12) 0.0000 0.19(3) Uani 1 2 d S TU P . .
H2 H 0.7500 -0.8110 0.0000 0.231 Uiso 1 2 calc R U P . .
C4 C 0.332(10) -0.754(13) -0.139(12) 0.24(5) Uani 1 1 d D U . . .
H4A H 0.2697 -0.6786 -0.2123 0.353 Uiso 1 1 calc R U . . .
H4B H 0.3657 -0.8245 -0.2378 0.353 Uiso 1 1 calc R U . . .
H4C H 0.4157 -0.7057 -0.0626 0.353 Uiso 1 1 calc R U . . .
N1 N 0.2500 -0.833(18) 0.0000 0.28(5) Uani 1 2 d DS TU P . .
H1A H 0.3191 -0.8984 0.0833 0.330 Uiso 0.5 1 calc R U P . .
H1B H 0.1809 -0.8984 -0.0833 0.330 Uiso 0.5 1 calc R U P . .
C3 C 0.460(4) -0.986(6) 0.407(5) 0.15(3) Uani 1 1 d . U . . .
C1 C 0.531(10) -0.471(11) 0.52(2) 0.21(3) Uani 0.5 1 d D U P . .
H1 H 0.6082 -0.4096 0.5827 0.252 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.13(9) 2_656 ?
Er1 O1 2.13(9) . ?
Er1 O2 2.39(4) 2_656 ?
Er1 O2 2.39(4) . ?
Er1 O4 2.24(4) . ?
Er1 O4 2.24(4) 2_656 ?
Er1 O3 2.51(6) 2_656 ?
Er1 O3 2.51(6) . ?
Er1 C3 2.97(5) 4_635 ?
O1 C1 1.19(11) 3_646 ?
O1 C1 1.25(9) . ?
O2 C2 1.07(4) . ?
O4 C3 1.49(8) . ?
O3 C3 1.05(4) 3_636 ?
C2 O2 1.07(4) 2_655 ?
C2 H2 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 N1 1.40(2) . ?
N1 C4 1.40(2) 2 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
C3 Er1 2.97(5) 3_636 ?
C3 O3 1.05(4) 3_636 ?
C3 C3 1.35(7) 3_636 ?
C1 O1 1.19(11) 3_646 ?
C1 H1 0.9300 . ?

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 Er1 O1 90(6) 2_656 . ?
O1 Er1 O2 73.4(17) 2_656 . ?
O1 Er1 O2 75.0(16) . . ?
O1 Er1 O2 73.4(17) . 2_656 ?
O1 Er1 O2 75.0(16) 2_656 2_656 ?
O1 Er1 O4 145(3) 2_656 . ?
O1 Er1 O4 73(3) . . ?
O1 Er1 O4 73(3) 2_656 2_656 ?
O1 Er1 O4 145(3) . 2_656 ?
O1 Er1 O3 103(3) . . ?
O1 Er1 O3 103(3) 2_656 2_656 ?
O1 Er1 O3 146.3(19) 2_656 . ?
O1 Er1 O3 146.3(19) . 2_656 ?
O1 Er1 C3 93(3) 2_656 4_635 ?
O1 Er1 C3 165.6(15) . 4_635 ?
O2 Er1 O2 135(3) . 2_656 ?
O2 Er1 O3 79.1(19) 2_656 . ?
O2 Er1 O3 139.9(16) . . ?
O2 Er1 O3 79.1(19) . 2_656 ?
O2 Er1 O3 139.9(16) 2_656 2_656 ?
O2 Er1 C3 121.0(14) 2_656 4_635 ?
O2 Er1 C3 92.5(14) . 4_635 ?
O4 Er1 O2 73.2(19) . . ?
O4 Er1 O2 125.4(13) 2_656 . ?
O4 Er1 O2 125.4(13) . 2_656 ?
O4 Er1 O2 73.2(19) 2_656 2_656 ?
O4 Er1 O4 136(5) . 2_656 ?
O4 Er1 O3 68.1(19) . . ?
O4 Er1 O3 68.1(19) 2_656 2_656 ?
O4 Er1 O3 79.1(18) 2_656 . ?
O4 Er1 O3 79.1(18) . 2_656 ?
O4 Er1 C3 48.4(19) 2_656 4_635 ?
O4 Er1 C3 97(2) . 4_635 ?
O3 Er1 O3 83(3) . 2_656 ?
O3 Er1 C3 82.1(18) . 4_635 ?
O3 Er1 C3 19.8(8) 2_656 4_635 ?
C1 O1 Er1 166(10) 3_646 . ?
C1 O1 Er1 154(7) . . ?
C1 O1 C1 38(10) 3_646 . ?
C2 O2 Er1 138(6) . . ?
C3 O4 Er1 119(3) . . ?
C3 O3 Er1 106(4) 3_636 . ?
O2 C2 O2 142(10) . 2_655 ?
O2 C2 H2 109.2 2_655 . ?
O2 C2 H2 109.2 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
C4 N1 C4 121(10) . 2 ?
C4 N1 H1A 107.1 . . ?
C4 N1 H1A 107.1 2 . ?
C4 N1 H1B 107.1 . . ?
C4 N1 H1B 107.1 2 . ?
H1A N1 H1B 106.8 . . ?
O4 C3 Er1 167(2) . 3_636 ?
O3 C3 Er1 54(4) 3_636 3_636 ?
O3 C3 O4 113(4) 3_636 . ?
O3 C3 C3 143(7) 3_636 3_636 ?
C3 C3 Er1 89(5) 3_636 3_636 ?
C3 C3 O4 104(5) 3_636 . ?
O1 C1 O1 142(10) 3_646 . ?
O1 C1 H1 108.9 3_646 . ?
O1 C1 H1 108.9 . . ?

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 O1 C1 O1 -168(12) . . . 3_646 ?
Er1 O2 C2 O2 -175(4) . . . 2_655 ?
Er1 O4 C3 Er1 -171(8) . . . 3_636 ?
Er1 O4 C3 O3 175(4) . . . 3_636 ?
Er1 O4 C3 C3 -5(4) . . . 3_636 ?
C1 O1 C1 O1 0.000(17) 3_646 . . 3_646 ?

_olex2_exptl_crystal_mounting_method 'in DAC with PTM of 4:1 methanol:ethanol'
_olex2_submission_original_sample_id 24_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_03_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320844'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_03_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.314 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_03_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.70 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT911_03_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        537 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-12-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        03_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   9.1533(2)
_cell_length_b                   8.9945(16)
_cell_length_c                   13.1812(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.7470(10)
_cell_angle_gamma                90
_cell_volume                     1077.68(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2841
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.596
_cell_measurement_theta_min      1.759
_shelx_estimated_absorpt_T_max   0.703
_shelx_estimated_absorpt_T_min   0.535
_exptl_absorpt_coefficient_mu    2.826
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_preparation       'Solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.314
_diffrn_reflns_Laue_measured_fraction_max 0.180
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5265
_diffrn_reflns_point_group_measured_fraction_full 0.314
_diffrn_reflns_point_group_measured_fraction_max 0.180
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         25.596
_diffrn_reflns_theta_min         1.759
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.314
_diffrn_measured_fraction_theta_max 0.180
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                964
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1140
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0430P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0679
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 O3, C3, C4, O4, O6, O5
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
O5 \\sim O6 \\sim C4 \\sim C3 \\sim O4 \\sim O3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C2, O7, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C4, O4, C3, O3, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, N1, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_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 0.2500 0.28786(8) 0.7500 0.0228(4) Uani 1 2 d S T P . .
Er2 Er 0.7500 0.74604(6) 0.7500 0.0234(4) Uani 1 2 d S T P . .
O4 O 0.3453(3) 0.4885(10) 0.66260(17) 0.045(4) Uani 1 1 d . U . . .
O3 O 0.4697(4) 0.3809(14) 0.8406(2) 0.064(4) Uani 1 1 d . U . . .
O6 O 0.5252(4) 0.6590(13) 0.6620(2) 0.050(3) Uani 1 1 d . U . . .
C3 C 0.5345(5) 0.4873(12) 0.8020(3) 0.046(3) Uani 1 1 d . U . . .
O1 O 0.0753(5) 0.1038(15) 0.7322(3) 0.075(5) Uani 1 1 d . U . . .
C4 C 0.4617(5) 0.5523(13) 0.6986(2) 0.040(3) Uani 1 1 d . U . . .
C2 C 0.2715(5) 0.2445(12) 0.5016(2) 0.047(4) Uani 1 1 d . U . . .
H2 H 0.2955 0.3446 0.4976 0.056 Uiso 1 1 calc R U . . .
O2 O 0.2550(5) 0.1721(11) 0.4201(2) 0.048(4) Uani 1 1 d . U . . .
O7 O 0.2585(6) 0.1933(11) 0.5866(2) 0.050(4) Uani 1 1 d . U . . .
C6 C 0.3233(8) -0.230(2) 0.4252(7) 0.096(8) Uani 1 1 d . U . . .
H6A H 0.3594 -0.1957 0.3637 0.143 Uiso 1 1 calc R U . . .
H6B H 0.3075 -0.3351 0.4213 0.143 Uiso 1 1 calc R U . . .
H6C H 0.3941 -0.2072 0.4828 0.143 Uiso 1 1 calc R U . . .
O5 O 0.6526(3) 0.5482(11) 0.83703(18) 0.063(4) Uani 1 1 d . U . . .
C1 C 0.0273(6) -0.0054(18) 0.7680(3) 0.063(5) Uani 1 1 d . U . . .
H1 H 0.0892 -0.0558 0.8176 0.075 Uiso 1 1 calc R U . . .
O8 O -0.0928(4) -0.0555(13) 0.7458(2) 0.065(5) Uani 1 1 d . U . . .
N1 N 0.1795(4) -0.1522(14) 0.4375(2) 0.073(7) Uani 1 1 d . U . . .
H1A H 0.1919 -0.0458 0.4300 0.088 Uiso 1 1 calc R U . . .
H1B H 0.1048 -0.1850 0.3838 0.088 Uiso 1 1 calc R U . . .
C5 C 0.1302(8) -0.1826(18) 0.5363(4) 0.074(8) Uani 1 1 d . U . . .
H5A H 0.0255 -0.1694 0.5317 0.111 Uiso 1 1 calc R U . . .
H5B H 0.1777 -0.1154 0.5863 0.111 Uiso 1 1 calc R U . . .
H5C H 0.1547 -0.2831 0.5561 0.111 Uiso 1 1 calc R U . . .


_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 O4 2.363(7) 2_556 ?
Er1 O4 2.363(7) . ?
Er1 O3 2.368(5) 2_556 ?
Er1 O3 2.368(5) . ?
Er1 O1 2.295(10) 2_556 ?
Er1 O1 2.295(10) . ?
Er1 O7 2.325(4) . ?
Er1 O7 2.325(4) 2_556 ?
Er2 O6 2.373(5) . ?
Er2 O6 2.373(5) 2_656 ?
Er2 O2 2.355(4) 3_666 ?
Er2 O2 2.355(4) 4_666 ?
Er2 O5 2.349(7) 2_656 ?
Er2 O5 2.349(8) . ?
Er2 O8 2.297(9) 2_566 ?
Er2 O8 2.297(9) 1_665 ?
O4 C4 1.253(8) . ?
O3 C3 1.264(12) . ?
O6 C4 1.249(13) . ?
C3 C4 1.559(9) . ?
C3 O5 1.251(8) . ?
O1 C1 1.196(17) . ?
C2 H2 0.9300 . ?
C2 O2 1.251(8) . ?
C2 O7 1.230(6) . ?
O2 Er2 2.355(4) 3_666 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 N1 1.515(12) . ?
C1 H1 0.9300 . ?
C1 O8 1.193(8) . ?
O8 Er2 2.297(9) 1_445 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
N1 C5 1.454(8) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
O4 Er1 O4 80.4(3) 2_556 . ?
O4 Er1 O3 79.9(3) 2_556 . ?
O4 Er1 O3 79.9(3) . 2_556 ?
O4 Er1 O3 68.6(2) 2_556 2_556 ?
O4 Er1 O3 68.6(2) . . ?
O3 Er1 O3 138.6(6) . 2_556 ?
O1 Er1 O4 142.56(14) 2_556 2_556 ?
O1 Er1 O4 108.0(3) 2_556 . ?
O1 Er1 O4 142.57(14) . . ?
O1 Er1 O4 108.0(3) . 2_556 ?
O1 Er1 O3 147.9(3) 2_556 2_556 ?
O1 Er1 O3 70.3(4) 2_556 . ?
O1 Er1 O3 70.3(4) . 2_556 ?
O1 Er1 O3 147.9(3) . . ?
O1 Er1 O1 87.6(5) . 2_556 ?
O1 Er1 O7 74.5(2) . 2_556 ?
O1 Er1 O7 74.9(2) . . ?
O1 Er1 O7 74.9(2) 2_556 2_556 ?
O1 Er1 O7 74.5(2) 2_556 . ?
O7 Er1 O4 76.9(3) 2_556 2_556 ?
O7 Er1 O4 141.8(2) . 2_556 ?
O7 Er1 O4 76.9(3) . . ?
O7 Er1 O4 141.8(2) 2_556 . ?
O7 Er1 O3 118.53(18) . . ?
O7 Er1 O3 77.3(2) . 2_556 ?
O7 Er1 O3 77.3(2) 2_556 . ?
O7 Er1 O3 118.53(18) 2_556 2_556 ?
O7 Er1 O7 137.1(5) . 2_556 ?
O6 Er2 O6 141.5(5) . 2_656 ?
O2 Er2 O6 73.68(19) 4_666 2_656 ?
O2 Er2 O6 73.68(19) 3_666 . ?
O2 Er2 O6 119.16(16) 4_666 . ?
O2 Er2 O6 119.17(15) 3_666 2_656 ?
O2 Er2 O2 143.5(5) 4_666 3_666 ?
O5 Er2 O6 82.4(2) 2_656 . ?
O5 Er2 O6 68.4(2) . . ?
O5 Er2 O6 82.4(2) . 2_656 ?
O5 Er2 O6 68.4(2) 2_656 2_656 ?
O5 Er2 O2 74.8(3) 2_656 3_666 ?
O5 Er2 O2 137.4(2) . 3_666 ?
O5 Er2 O2 74.8(3) . 4_666 ?
O5 Er2 O2 137.4(2) 2_656 4_666 ?
O5 Er2 O5 81.5(4) 2_656 . ?
O8 Er2 O6 76.0(3) 1_665 2_656 ?
O8 Er2 O6 138.9(3) 2_566 2_656 ?
O8 Er2 O6 76.0(3) 2_566 . ?
O8 Er2 O6 138.9(2) 1_665 . ?
O8 Er2 O2 71.1(2) 2_566 4_666 ?
O8 Er2 O2 71.1(2) 1_665 3_666 ?
O8 Er2 O2 80.7(2) 1_665 4_666 ?
O8 Er2 O2 80.7(2) 2_566 3_666 ?
O8 Er2 O5 151.06(12) 1_665 . ?
O8 Er2 O5 107.6(3) 2_566 . ?
O8 Er2 O5 151.06(12) 2_566 2_656 ?
O8 Er2 O5 107.6(3) 1_665 2_656 ?
O8 Er2 O8 78.0(4) 1_665 2_566 ?
C4 O4 Er1 120.7(4) . . ?
C3 O3 Er1 118.4(3) . . ?
C4 O6 Er2 118.8(3) . . ?
O3 C3 C4 117.6(6) . . ?
O5 C3 O3 127.5(5) . . ?
O5 C3 C4 114.9(8) . . ?
C1 O1 Er1 146.7(4) . . ?
O4 C4 C3 114.6(8) . . ?
O6 C4 O4 128.3(5) . . ?
O6 C4 C3 117.1(6) . . ?
O2 C2 H2 117.5 . . ?
O7 C2 H2 117.5 . . ?
O7 C2 O2 124.9(10) . . ?
C2 O2 Er2 129.9(7) . 3_666 ?
C2 O7 Er1 136.4(7) . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
C3 O5 Er2 120.8(5) . . ?
O1 C1 H1 117.1 . . ?
O8 C1 O1 125.7(10) . . ?
O8 C1 H1 117.1 . . ?
C1 O8 Er2 148.1(10) . 1_445 ?
C6 N1 H1A 109.2 . . ?
C6 N1 H1B 109.2 . . ?
H1A N1 H1B 107.9 . . ?
C5 N1 C6 112.0(8) . . ?
C5 N1 H1A 109.2 . . ?
C5 N1 H1B 109.2 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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 C4 O6 -179.9(8) . . . . ?
Er1 O4 C4 C3 0.5(10) . . . . ?
Er1 O3 C3 C4 1.7(11) . . . . ?
Er1 O3 C3 O5 -178.1(7) . . . . ?
Er1 O1 C1 O8 160.9(11) . . . . ?
Er2 O6 C4 O4 -178.0(7) . . . . ?
Er2 O6 C4 C3 1.6(11) . . . . ?
O3 C3 C4 O4 -1.5(12) . . . . ?
O3 C3 C4 O6 178.8(6) . . . . ?
O3 C3 O5 Er2 -179.8(8) . . . . ?
O1 C1 O8 Er2 164.1(10) . . . 1_445 ?
C4 C3 O5 Er2 0.4(10) . . . . ?
O2 C2 O7 Er1 -170.6(5) . . . . ?
O7 C2 O2 Er2 172.7(5) . . . 3_666 ?
O5 C3 C4 O4 178.3(6) . . . . ?
O5 C3 C4 O6 -1.3(12) . . . . ?

_olex2_exptl_crystal_mounting_method 
'in diamond anvil cell with pressure transmitting medium of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 03_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_18_dma01
_database_code_depnum_ccdc_archive 'CCDC 2320850'
loop_
_audit_author_name
_audit_author_address
'Thomas Hitchings'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_18_dma01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.319 Why?
RESPONSE: Conical shaped opening of the diamond anvil cell limits maximum values of 2theta and completeness.
;
_vrf_PLAT088_18_dma01            
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.66 Note
RESPONSE: Atoms refined anisotropically, low data completeness.
;
_vrf_PLAT241_18_dma01            
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O1 Check
RESPONSE: no absorption correction applied, Er is a heavy element.
;
_vrf_PLAT242_18_dma01            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Er1 Check
RESPONSE: No absorption correction applied, Er is a heavy element.
;
_vrf_PLAT342_18_dma01            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.
RESPONSE: A combination of heavy and light elements is present in the structure, and only a single C-C bond is present.
;
_vrf_PLAT911_18_dma01            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        144 Report
RESPONSE: limited accessibility to reciprocal space.
;
# Added during the CSD deposition process: Wednesday 20 December 2023 12:34 PM
# end Validation Reply Form

_audit_creation_date             2023-07-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelxl_version_number           2013-4
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        18_DMA01
_chemical_formula_moiety         'C4 H2 Er O8, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_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 -0.0004 0.0007 '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 -0.9218 2.6017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0004 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0006 0.0026 '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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/a 1'
_space_group_name_Hall           '-P 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'-x, -y, -z'
'x-1/2, -y, z'

_cell_length_a                   9.1025(11)
_cell_length_b                   8.913(8)
_cell_length_c                   6.5273(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.442(7)
_cell_angle_gamma                90
_cell_volume                     526.2(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2256
_cell_measurement_temperature    300
_cell_measurement_theta_max      20.332
_cell_measurement_theta_min      2.147
_shelx_estimated_absorpt_T_max   0.698
_shelx_estimated_absorpt_T_min   0.528
_exptl_absorpt_coefficient_mu    2.894
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.470
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             370
_exptl_crystal_preparation       'Solvothermal synthesis,Magnetic properties'
_exptl_crystal_recrystallization_method 'crash cooling'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.134
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.319
_diffrn_reflns_Laue_measured_fraction_max 0.280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2338
_diffrn_reflns_point_group_measured_fraction_full 0.319
_diffrn_reflns_point_group_measured_fraction_max 0.280
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         20.332
_diffrn_reflns_theta_min         2.147
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.319
_diffrn_measured_fraction_theta_max 0.280
_diffrn_measurement_device_type  I19-2
_diffrn_measurement_method       Shutterless
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   Diamond
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                362
_reflns_number_total             453
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         453
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0503
_refine_ls_restrained_S_all      1.146
_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)+(0.0884P)²+1.3333P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1515
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C1
 1.3 with sigma of 0.1
 C4-N1
 1.4 with sigma of 0.02
 O1-C1 \\sim O1-C1_$2
 with sigma of 0.01
3. Restrained planarity
 O4, C3, C3_$1, O3, O4_$1, O3_$1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O1) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C3, O3, O3, C3, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C1(0.5) H1(0.5)
7.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_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 0.7500 -0.7705(3) 0.5000 0.0583(17) Uani 1 2 d S T P . .
O1 O 0.580(4) -0.600(10) 0.483(4) 0.156(15) Uani 1 1 d D U . . .
O2 O 0.753(3) -0.682(6) 0.167(2) 0.15(2) Uani 1 1 d . U . . .
O4 O 0.535(3) -0.858(7) 0.319(3) 0.12(3) Uani 1 1 d . U . . .
O3 O 0.651(2) -0.977(6) 0.680(3) 0.12(3) Uani 1 1 d . . . . .
C2 C 0.7500 -0.727(10) 0.0000 0.10(7) Uani 1 2 d S T P . .
H2 H 0.7500 -0.8315 0.0000 0.114 Uiso 1 2 calc R U P . .
C4 C 0.354(9) -0.739(17) -0.121(12) 0.21(4) Uani 1 1 d D U . . .
H4A H 0.4419 -0.7118 -0.0334 0.321 Uiso 1 1 calc R U . . .
H4B H 0.3130 -0.6518 -0.1915 0.321 Uiso 1 1 calc R U . . .
H4C H 0.3784 -0.8122 -0.2198 0.321 Uiso 1 1 calc R U . . .
N1 N 0.2500 -0.80(2) 0.0000 0.25(4) Uani 1 2 d DS TU P . .
H1A H 0.3087 -0.8666 0.0948 0.304 Uiso 0.5 1 calc R U P . .
H1B H 0.1913 -0.8666 -0.0948 0.304 Uiso 0.5 1 calc R U P . .
C3 C 0.463(3) -0.970(4) 0.398(3) 0.08(3) Uani 1 1 d . U . . .
C1 C 0.532(12) -0.476(10) 0.52(2) 0.15(2) Uani 0.5 1 d D U P . .
H1 H 0.6125 -0.4147 0.5627 0.183 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.17(6) 2_656 ?
Er1 O1 2.17(6) . ?
Er1 O2 2.32(2) 2_656 ?
Er1 O2 2.32(2) . ?
Er1 O4 2.31(3) . ?
Er1 O4 2.31(3) 2_656 ?
Er1 O3 2.41(4) . ?
Er1 O3 2.41(4) 2_656 ?
O1 C1 1.22(7) 3_646 ?
O1 C1 1.22(7) . ?
O2 C2 1.16(3) . ?
O4 C3 1.33(5) . ?
O3 C3 1.20(4) 3_636 ?
C2 O2 1.16(3) 2_655 ?
C2 H2 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 N1 1.41(2) . ?
N1 C4 1.41(2) 2 ?
N1 H1A 0.9700 . ?
N1 H1B 0.9700 . ?
C3 O3 1.20(4) 3_636 ?
C3 C3 1.52(4) 3_636 ?
C1 O1 1.22(7) 3_646 ?
C1 H1 0.9300 . ?

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 Er1 O1 91(4) 2_656 . ?
O1 Er1 O2 74.0(11) . 2_656 ?
O1 Er1 O2 74.0(11) 2_656 . ?
O1 Er1 O2 78.2(12) 2_656 2_656 ?
O1 Er1 O2 78.2(12) . . ?
O1 Er1 O4 145.7(18) 2_656 . ?
O1 Er1 O4 70(2) 2_656 2_656 ?
O1 Er1 O4 70(2) . . ?
O1 Er1 O4 145.7(18) . 2_656 ?
O1 Er1 O3 144.6(12) . 2_656 ?
O1 Er1 O3 105(2) . . ?
O1 Er1 O3 105(2) 2_656 2_656 ?
O1 Er1 O3 144.6(12) 2_656 . ?
O2 Er1 O2 140(2) 2_656 . ?
O2 Er1 O3 139.7(12) . . ?
O2 Er1 O3 76.0(14) 2_656 . ?
O2 Er1 O3 139.7(12) 2_656 2_656 ?
O2 Er1 O3 76.0(14) . 2_656 ?
O4 Er1 O2 119.9(9) . 2_656 ?
O4 Er1 O2 74.6(12) . . ?
O4 Er1 O2 74.6(11) 2_656 2_656 ?
O4 Er1 O2 119.9(9) 2_656 . ?
O4 Er1 O4 140(3) . 2_656 ?
O4 Er1 O3 80.5(13) 2_656 . ?
O4 Er1 O3 69.4(12) . . ?
O4 Er1 O3 80.5(13) . 2_656 ?
O4 Er1 O3 69.4(12) 2_656 2_656 ?
O3 Er1 O3 80.7(18) . 2_656 ?
C1 O1 Er1 153(7) . . ?
C1 O1 Er1 168(8) 3_646 . ?
C1 O1 C1 36(10) 3_646 . ?
C2 O2 Er1 139(4) . . ?
C3 O4 Er1 118.9(18) . . ?
C3 O3 Er1 116(2) 3_636 . ?
O2 C2 O2 139(7) . 2_655 ?
O2 C2 H2 110.5 2_655 . ?
O2 C2 H2 110.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
C4 N1 C4 134(10) . 2 ?
C4 N1 H1A 103.6 2 . ?
C4 N1 H1A 103.6 . . ?
C4 N1 H1B 103.6 2 . ?
C4 N1 H1B 103.6 . . ?
H1A N1 H1B 105.3 . . ?
O4 C3 C3 114(4) . 3_636 ?
O3 C3 O4 125(2) 3_636 . ?
O3 C3 C3 121(5) 3_636 3_636 ?
O1 C1 O1 144(10) 3_646 . ?
O1 C1 H1 107.9 3_646 . ?
O1 C1 H1 107.9 . . ?

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 O1 C1 O1 -166(9) . . . 3_646 ?
Er1 O2 C2 O2 177(3) . . . 2_655 ?
Er1 O4 C3 O3 179(2) . . . 3_636 ?
Er1 O4 C3 C3 -2(3) . . . 3_636 ?
C1 O1 C1 O1 0.000(17) 3_646 . . 3_646 ?

_olex2_exptl_crystal_mounting_method 
'in diamond anvil cell, with pressure transmitting media of 4:1 methanol:ethanol.'
_olex2_submission_original_sample_id 18_DMA01
_olex2_submission_special_instructions 'No special instructions were received'
