Negative linear compressibility exhibited by the hybrid perovskite [(NH<sub>2</sub>)<sub>3</sub>C]Er(HCO<sub>2</sub>)<sub>2</sub>(C<sub>2</sub>O<sub>4</sub>).
Hitchings, Thomas J.; Scatena, Rebecca; Allan, David R.; Cairns, Andrew B.; Saines, Paul J.; Chemical communications (Cambridge, England) 60 (2024) 3271–3274; doi:10.1039/d3cc06208b

data_7132753
_publ_section_title
;
 Negative linear compressibility exhibited by the hybrid perovskite
 [(NH<sub>2</sub>)<sub>3</sub>C]Er(HCO<sub>2</sub>)<sub>2</sub>(C<sub>2</sub>O<sub>4</sub>).
;
_journal_issue                   24
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3271
_journal_page_last               3274
_journal_paper_doi               10.1039/d3cc06208b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C4 H2 Er O8, C H6 N3'
_chemical_formula_sum            'C5 H8 Er N3 O8'
_chemical_formula_weight         405.40
_chemical_name_common            'Guanadinium Erbium(III) Formate Oxalate'
_chemical_name_systematic        36_GUA03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.736(8)
_cell_length_b                   6.479(5)
_cell_length_c                   19.71(12)
_cell_measurement_reflns_used    1994
_cell_measurement_temperature    300
_cell_measurement_theta_max      15.601
_cell_measurement_theta_min      2.149
_cell_volume                     988(6)
_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)'
_diffrn_ambient_temperature      300
_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_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_source                   Diamond
_exptl_absorpt_coefficient_mu    3.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.726
_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
_refine_diff_density_max         1.457
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.350
_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_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.1159
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2877
_refine_ls_wR_factor_ref         0.3100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                223
_reflns_number_total             393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06208b2.cif
_cod_data_source_block           36_gua03
_cod_depositor_comments
'Adding full bibliography for 7132745--7132763.cif.'
_cod_database_code               7132753
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.742
_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)
;
_shelx_res_checksum              68358
_shelx_hkl_checksum              65618
_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'