Disorder‒order transitions in the perovskite metal‒organic frameworks [(CH3)2NH2][M(HCOO)3] at high pressure
Collings, Ines; Bykov, Maxim; Bykova, Elena; Hanfland, Michael; van Smaalen, Sander; Dubrovinsky, Leonid; Dubrovinskaia, Natalia; CrystEngComm  (2018) –; doi:10.1039/C8CE00617B

data_7230777
_publ_section_title
;
 Disorder--order transitions in the perovskite metal--organic frameworks
 [(CH3)2NH2][M(HCOO)3] at high pressure
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE00617B
_journal_year                    2018
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.0225(6)
_cell_length_b                   8.0225(6)
_cell_length_c                   21.1076(16)
_cell_measurement_reflns_used    175
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.7640
_cell_measurement_theta_min      2.9390
_cell_volume                     1176.49(15)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_pressure         '3.94 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7
_diffrn_measured_fraction_theta_full 0.731
_diffrn_measured_fraction_theta_max 0.466
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.731
_diffrn_reflns_Laue_measured_fraction_max 0.466
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            748
_diffrn_reflns_point_group_measured_fraction_full 0.731
_diffrn_reflns_point_group_measured_fraction_max 0.466
_diffrn_reflns_theta_full        14.280
_diffrn_reflns_theta_max         19.349
_diffrn_reflns_theta_min         2.937
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         270
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0470P)^2^+6.9966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                214
_reflns_number_total             270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00617b2.cif
_cod_data_source_block           DMAFeF_c2_p04
_cod_original_cell_volume        1176.49(19)
_cod_database_code               7230777
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              31641