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_7132761
_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        24_DMA01
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2ya'
_space_group_name_H-M_alt        'P 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-12-20 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.131(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0471(15)
_cell_length_b                   8.792(11)
_cell_length_c                   6.4339(9)
_cell_measurement_reflns_used    1626
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      17.138
_cell_measurement_theta_min      2.177
_cell_volume                     508.8(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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.00
_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_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_source                   Diamond
_exptl_absorpt_coefficient_mu    2.993
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.555
_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
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.095
_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_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0461
_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^)+(0.1157P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                236
_reflns_number_total             306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06208b2.cif
_cod_data_source_block           24_dma01
_cod_depositor_comments
'Adding full bibliography for 7132745--7132763.cif.'
_cod_original_cell_volume        508.9(7)
_cod_database_code               7132761
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.690
_shelx_estimated_absorpt_t_min   0.518
_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)
;
_shelx_res_checksum              67236
_shelx_hkl_checksum              74201
_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'