Tunable hybrid perovskites with Narrow bandgap and Multistage phase transition properties: 2,2-difluoroethylamine·Antimony Hexabromide
Song, Ning; Chen, Shao-Peng; Fan, Xiao-Wei; Tan, Yu-Hui; Tang, Yun Zhi; Wang, Li Juan; Liao, Juan; Sun, Zhen; CrystEngComm  (2022) –; doi:10.1039/D2CE00438K

data_7244866
_publ_section_title
;
 Tunable hybrid perovskites with Narrow bandgap and Multistage phase
 transition properties: 2,2-difluoroethylamine&#x00B7;Antimony Hexabromide
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00438K
_journal_year                    2022
_chemical_formula_moiety         'Br6 Sb, C2 H5 F3 N, 2(C2 H6 F2 N)'
_chemical_formula_sum            'C6 H14 Br6 F7 N3 Sb'
_chemical_formula_weight         862.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-02 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3766(5)
_cell_length_b                   21.5176(8)
_cell_length_c                   8.0757(3)
_cell_measurement_reflns_used    5957
_cell_measurement_temperature    292.99(10)
_cell_measurement_theta_max      29.7830
_cell_measurement_theta_min      2.6900
_cell_volume                     2150.68(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -54.00 -29.00   0.50    3.00    --    6.16 -16.00-172.00   50
  2  \w    -19.00  28.00   0.50    3.00    --   -5.69 -99.00 -60.00   94
  3  \w    -20.00  39.00   0.50    3.00    --    6.16 -99.00 -30.00  118
  4  \w     -4.00  22.00   0.50    3.00    --    6.16 -99.00 120.00   52
  5  \w    -21.00  22.00   0.50    3.00    --    6.16 -16.00-172.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0056021000
_diffrn_orient_matrix_UB_12      -0.0564701000
_diffrn_orient_matrix_UB_13      -0.0009200000
_diffrn_orient_matrix_UB_21      0.0317113000
_diffrn_orient_matrix_UB_22      0.0094010000
_diffrn_orient_matrix_UB_23      0.0191553000
_diffrn_orient_matrix_UB_31      -0.0070365000
_diffrn_orient_matrix_UB_32      -0.0027121000
_diffrn_orient_matrix_UB_33      0.0857143000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11862
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.69
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.097
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2046
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+3.6882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                1733
_reflns_number_total             2046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2ce00438k2.cif
_cod_data_source_block           csp_1_t293k
_cod_database_code               7244866
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 F1-C1
 2.4 with sigma of 0.02
 F1-C2
 1.25 with sigma of 0.02
3. Others
 Fixed Sof: H2a(0.5) H2b(0.5) H2c(0.5) H4a(0.5) H4b(0.5) H3a(0.5) H3b(0.5)
 H3c(0.5) H6a(0.5) H6b(0.5) H1a(0.5) H1b(0.5) H1c(0.5) H1d(0.5) H1e(0.5)
4.a Ternary CH refined with riding coordinates:
 C5(H5), C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C6(H6a,H6b), C1(H1d,H1e)
4.c Idealised Me refined as rotating group:
 N2(H2a,H2b,H2c), N3(H3a,H3b,H3c), N1(H1a,H1b,H1c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.292
_oxdiff_exptl_absorpt_empirical_full_min 0.533