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_7132757
_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, C2 H8 N'
_chemical_formula_sum            'C6 H10 Er N O8'
_chemical_formula_weight         391.41
_chemical_name_common            'Dimethylammonium Erbium(III) Formate Oxalate'
_chemical_name_systematic        12_DMA01
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-19
_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                 96.440(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1263(6)
_cell_length_b                   8.963(4)
_cell_length_c                   13.1305(7)
_cell_measurement_reflns_used    2382
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      21.226
_cell_measurement_theta_min      1.769
_cell_volume                     1067.3(5)
_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)'
_diffrn_ambient_temperature      300.00
_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_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_source                   Diamond
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.436
_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
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.136
_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_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0921P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                633
_reflns_number_total             1016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06208b2.cif
_cod_data_source_block           12_dma01
_cod_depositor_comments
'Adding full bibliography for 7132745--7132763.cif.'
_cod_database_code               7132757
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.532
_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)
;
_shelx_res_checksum              99421
_shelx_hkl_checksum              11540
_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'