Principles of Melting in Hybrid Organic-Inorganic Perovskite and Polymorphic ABX3 Structures
Shaw, Bikash Kumar; Bennett, Thomas Douglas; Castillo Blas, Celia; Thorne, Michael Francis; Gómez, María Laura Ríos; Forrest, Thomas; Keen, David A.; Diaz-Lopez, Maria; Chater, Philip A.; McHugh, Lauren Nicole; Chemical Science  (2022) –; doi:10.1039/D1SC07080K

data_1566080
_publ_section_title
;
 Principles of Melting in Hybrid Organic-Inorganic Perovskite and
 Polymorphic ABX3 Structures
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC07080K
_journal_year                    2022
_chemical_formula_moiety         '(C20 H44 N1), (Fe1 C6 N9)'
_chemical_formula_sum            'C26 H44 Fe N10'
_chemical_formula_weight         552.56
_chemical_name_common
;
Tetrapentylammonium cobalt(II) dicyanamide
;
_chemical_name_systematic        '[TPnA][Fe(Dca)3]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-31 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1007(6)
_cell_length_b                   11.6128(5)
_cell_length_c                   20.0929(8)
_cell_measurement_reflns_used    2464
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      64.1490
_cell_measurement_theta_min      4.0250
_cell_volume                     3056.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9351
_diffrn_measured_fraction_theta_max 0.9921
_diffrn_measurement_details
;
  1 omega  -53.00   17.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      -51.2500   30.0000  -90.0000 70

  2 omega  -18.00   12.00   1.0000   16.4900
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -180.0000 30

  3 omega   33.00   80.00   1.0000   16.4900
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -30.0000 47

  4 omega   67.00  122.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -       51.2500  153.0000 -142.0000 55

  5 omega  121.00  147.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000 -120.0000 26

  6 omega  108.00  134.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000   43.0000  -90.0000 26

  7 omega  146.00  172.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000   43.0000  -90.0000 26

  8 omega  119.00  145.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000   43.0000    0.0000 26

  9 omega   64.00  101.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000   43.0000    0.0000 37

 10 omega   37.00   73.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000   30.0000 36

 11 omega   41.00   89.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000    0.0000 48

 12 omega   42.00   67.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000   90.0000 25

 13 omega   77.00  106.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -153.0000  176.0000 29

 14 omega   24.00   50.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -153.0000  176.0000 26

 15 omega   20.00   70.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000   30.0000 50

 16 omega   25.00   59.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  -30.0000 34

 17 omega   33.00   88.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000  -90.0000 55

 18 omega   25.00   66.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000 -150.0000 41

 19 omega   22.00   68.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  150.0000 46

 20 omega   43.00   71.00   1.0000   16.4900
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  150.0000 28

 21 omega -132.00  -25.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      -51.2500  -77.0000  150.0000 107

;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1112732000
_diffrn_orient_matrix_UB_12      -0.0425234000
_diffrn_orient_matrix_UB_13      -0.0035041000
_diffrn_orient_matrix_UB_21      0.0354363000
_diffrn_orient_matrix_UB_22      0.1086637000
_diffrn_orient_matrix_UB_23      0.0374462000
_diffrn_orient_matrix_UB_31      -0.0139700000
_diffrn_orient_matrix_UB_32      -0.0630051000
_diffrn_orient_matrix_UB_33      0.0668334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6312
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         64.3769
_diffrn_reflns_theta_min         2.1989
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       tetrahedral
_exptl_crystal_F_000             1184.7
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2546
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0609P)^2^+0.7873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2066
_reflns_number_total             2546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc07080k2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3056.9(2)
_cod_original_formula_sum        'C26 H44 Fe1 N10'
_cod_database_code               1566080
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 93.51
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              33789
_shelx_hkl_checksum              15981