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_7132746
_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        07_GUA04
_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             2023-12-15
_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                   8.1956(2)
_cell_length_b                   6.53400(18)
_cell_length_c                   19.322(5)
_cell_measurement_reflns_used    2326
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.972
_cell_measurement_theta_min      2.131
_cell_volume                     1034.7(3)
_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 0.381
_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_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_source                   Diamond
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.602
_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
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.100
_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_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0421P)^2^+1.0904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                484
_reflns_number_total             737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06208b2.cif
_cod_data_source_block           07_gua04
_cod_depositor_comments
'Adding full bibliography for 7132745--7132763.cif.'
_cod_database_code               7132746
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.678
_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)
;
_shelx_res_checksum              88325
_shelx_hkl_checksum              19939
_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'