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_7230776
_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         'C12 H12 Fe4 O24, 4(C2 H8 N)'
_chemical_formula_sum            'C20 H44 Fe4 N4 O24'
_chemical_formula_weight         947.96
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_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                90.26(6)
_cell_angle_beta                 91.72(9)
_cell_angle_gamma                99.47(10)
_cell_formula_units_Z            1
_cell_length_a                   10.763(11)
_cell_length_b                   8.256(7)
_cell_length_c                   7.985(6)
_cell_measurement_reflns_used    82
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.9750
_cell_measurement_theta_min      2.2180
_cell_volume                     699.5(11)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_pressure         '7.87 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7
_diffrn_measured_fraction_theta_full 0.828
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41119
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_Laue_measured_fraction_full 0.828
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1769
_diffrn_reflns_point_group_measured_fraction_full 0.559
_diffrn_reflns_point_group_measured_fraction_max 0.559
_diffrn_reflns_theta_full        12.511
_diffrn_reflns_theta_max         12.511
_diffrn_reflns_theta_min         1.476
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.251
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.13(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1769
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.314
_refine_ls_shift/su_mean         0.070
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2059
_reflns_Friedel_coverage         0.351
_reflns_Friedel_fraction_full    0.291
_reflns_Friedel_fraction_max     0.291
_reflns_number_gt                827
_reflns_number_total             1769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00617b2.cif
_cod_data_source_block           DMAFeFc6p03
_cod_database_code               7230776
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              43414