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_7244868
_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 H6 F2 N, 2(C2 H5 F2 N)'
_chemical_formula_sum            'C6 H18 Br6 F6 N3 Sb'
_chemical_formula_weight         847.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-03-02 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0374(9)
_cell_length_b                   12.3053(11)
_cell_length_c                   21.3990(15)
_cell_measurement_reflns_used    4363
_cell_measurement_temperature    232.97(10)
_cell_measurement_theta_max      29.5420
_cell_measurement_theta_min      2.6990
_cell_volume                     2116.4(3)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      232.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.734
_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     14.00  70.00   0.50    3.00    --   -5.69  17.00  -3.00  112
  2  \w    -21.00  28.00   0.50    3.00    --   -5.69 -99.00-120.00   98
  3  \w    -53.00  21.00   0.50    3.00    --    6.16 -77.00  60.00  148
;
_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      0.0008715000
_diffrn_orient_matrix_UB_12      0.0056659000
_diffrn_orient_matrix_UB_13      0.0568129000
_diffrn_orient_matrix_UB_21      -0.0201971000
_diffrn_orient_matrix_UB_22      0.0318175000
_diffrn_orient_matrix_UB_23      -0.0094311000
_diffrn_orient_matrix_UB_31      -0.0859721000
_diffrn_orient_matrix_UB_32      -0.0072229000
_diffrn_orient_matrix_UB_33      0.0027526000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1155
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.734
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12086
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.734
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.770
_diffrn_reflns_theta_min         2.707
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20653
_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    2.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.837
_refine_diff_density_min         -2.484
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4862
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1508
_refine_ls_R_factor_gt           0.1213
_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^)+(0.1292P)^2^+95.9600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3327
_refine_ls_wR_factor_ref         0.3475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3232
_reflns_number_total             4862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00438k2.cif
_cod_data_source_block           csp_1_t233k
_cod_database_code               7244868
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.702
_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
 N5-C2
 1.48 with sigma of 0.02
 Sb1-Br1 \\sim Sb1-Br1A
 with sigma of 0.02
 Sb1-Br2 \\sim Sb1-Br2A
 with sigma of 0.02
 Sb1-Br5 \\sim Sb1-Br5A
 with sigma of 0.02
 Sb1-Br4 \\sim Sb1-Br4A
 with sigma of 0.02
 Sb1-Br6 \\sim Sb1-Br6A
 with sigma of 0.02
 F4-C7 \\sim F4A-C7
 with sigma of 0.02
 F5-F6 \\sim F5-F6A
 with sigma of 0.02
 F6-C9 \\sim F6A-C9
 with sigma of 0.02
3. Others
 Sof(Br1A)=1-FVAR(1)
 Sof(Br1)=FVAR(1)
 Sof(Br5A)=1-FVAR(2)
 Sof(Br5)=FVAR(2)
 Sof(Br2A)=1-FVAR(3)
 Sof(Br2)=FVAR(3)
 Sof(Br4A)=1-FVAR(4)
 Sof(Br4)=FVAR(4)
 Sof(Br6A)=1-FVAR(5)
 Sof(Br6)=FVAR(5)
 Sof(F4A)=1-FVAR(6)
 Sof(F4)=FVAR(6)
 Sof(F6A)=1-FVAR(7)
 Sof(F6)=FVAR(7)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5D,H5E)
4.c Idealised Me refined as rotating group:
 N2(H2C,H2D,H2E), N5(H5A,H5B,H5C), N8(H8A,H8B,H8C)
;
_shelx_res_checksum              14117
_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 2.614
_oxdiff_exptl_absorpt_empirical_full_min 0.468