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_1566081
_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), (Co1 C6 N9)'
_chemical_formula_sum            'C26 H44 Co N10'
_chemical_formula_weight         555.73
_chemical_name_common
;
Tetrapentylammonium cobalt(II) dicyanamide
;
_chemical_name_systematic        '[TPnA][Co(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                   13.066(2)
_cell_length_b                   11.6026(19)
_cell_length_c                   19.926(4)
_cell_measurement_reflns_used    1573
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      63.5190
_cell_measurement_theta_min      3.8980
_cell_volume                     3020.8(9)
_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 0.9333
_diffrn_measured_fraction_theta_max 0.9965
_diffrn_measurement_details
;
  1 omega   70.00   96.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -       51.2500 -125.0000  -60.0000 26

  2 omega   89.00  126.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -89.0000  -60.0000 37

  3 omega   40.00   74.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000    0.0000 34

  4 omega   29.00   74.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000  -90.0000 45

  5 omega   32.00   73.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000 -150.0000 41

  6 omega   32.00   59.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -89.0000  -60.0000 27

  7 omega   28.00   85.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000   60.0000 57

  8 omega   40.00   69.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000   90.0000 29

  9 omega   36.00  128.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -11.0000  120.0000 92

 10 omega  150.00  175.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000   90.0000 25

 11 omega   82.00  113.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000   90.0000 31

 12 omega   74.00  131.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000    0.0000 57

 13 omega   48.00   83.00   1.0000   13.0300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 35

 14 omega   35.00   60.00   1.0000   13.0300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -120.0000 25

 15 omega   -3.00   52.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -       51.2500 -125.0000  -60.0000 55

 16 omega   32.00   78.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000  150.0000 46

 17 omega   38.00   85.00   1.0000   13.0300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  120.0000 47

 18 omega   73.00  114.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000 -180.0000 41

 19 omega -124.00  -44.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      -51.2500  -61.0000    0.0000 80

;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1038941000
_diffrn_orient_matrix_UB_12      -0.0061930000
_diffrn_orient_matrix_UB_13      -0.0366279000
_diffrn_orient_matrix_UB_21      0.0367143000
_diffrn_orient_matrix_UB_22      0.0920317000
_diffrn_orient_matrix_UB_23      -0.0501036000
_diffrn_orient_matrix_UB_31      0.0424803000
_diffrn_orient_matrix_UB_32      -0.0954148000
_diffrn_orient_matrix_UB_33      -0.0459703000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       15
_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       -23
_diffrn_reflns_number            2570
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         64.1699
_diffrn_reflns_theta_min         2.2173
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.69897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37216
_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            pink
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       tetrahedral
_exptl_crystal_F_000             1336.00
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2520
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0989P)^2^+2.9499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1720
_reflns_number_total             2520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc07080k2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_formula_sum        'C26 H44 Co1 N10'
_cod_database_code               1566081
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 93.33
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              4897
_shelx_hkl_checksum              84776