Organic-Inorganic Layered and Hollow Tin Bromide Perovskite with Tunable Broadband Emission.
Fu, Pengfei; Huang, Menglin; Shang, Yuequn; Yu, Na; Zhou, Hao-Long; Zhang, Yue-Biao; Chen, Shiyou; Gong, Jinkang; Ning, Zhijun; ACS applied materials & interfaces 10 (2018) 34363–34369; doi:10.1021/acsami.8b07673

data_4515366
_publ_section_title
;
 Organic-Inorganic Layered and Hollow Tin Bromide Perovskite with Tunable
 Broadband Emission.
;
_journal_issue                   40
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              34363
_journal_page_last               34369
_journal_paper_doi               10.1021/acsami.8b07673
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         'Br4 Sn, 4(Br), 3(C6 H18 N2), 0.13(H16 O8)'
_chemical_formula_sum            'C18 H51.74 Br8 N6 O Sn'
_chemical_formula_weight         1126.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2018-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.739(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9725(12)
_cell_length_b                   17.532(2)
_cell_length_c                   22.757(3)
_cell_measurement_reflns_used    5843
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.35
_cell_volume                     3974.2(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21954
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.592
_diffrn_reflns_theta_min         2.323
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.706
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5380
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_description       block
_exptl_crystal_F_000             2159
_refine_diff_density_max         1.812
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0936P)^2^+29.9148P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2578
_reflns_number_total             4125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b07673_si_002.cif
_cod_data_source_block           mo_snetoh3_0m
_cod_original_cell_volume        3974.2(9)
_cod_database_code               4515366
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N2-C5
 2.5 with sigma of 0.02
 C6-C4
 2.5 with sigma of 0.02
 C7-C9
 2.5 with sigma of 0.02
 C9-C9_$1
 1.5 with sigma of 0.01
 N4-C10 = C11-C10 = C12-C11
 1.45 with sigma of 0.01
 C11-N4
 2.5 with sigma of 0.02
 C12-C10
 2.5 with sigma of 0.02
 N3-C7 = C8-C7 = C9-C8 = N2-C4 = C5-C4 = C5-C6
 1.45 with sigma of 0.02
 C8-N3
 2.5 with sigma of 0.02
 N3-C7 = N4-C10
 1.48 with sigma of 0.0001
 C7-C8
 1.5 with sigma of 0.02
 C6_$2-C6_$3
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N3 \\sim C7 \\sim C8 \\sim C9 \\sim C12 \\sim C11 \\sim C10 \\sim N4: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N3, C7, C8, C9, C12, C11, C10, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(N4)=Sof(H4C)=Sof(H4D)=Sof(H4E)=1-FVAR(1)
 Sof(N3)=Sof(H3C)=Sof(H3D)=Sof(H3E)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=
 Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
 Fixed Sof: O1(0.25) H1F(0.25) H1G(0.25) O2(0.25) H2F(0.25) H2G(0.25)
7.a Riding coordinates:
 N3(H3C,H3D,H3E), O1(H1F,H1G), O2(H2F,H2G)
7.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C1(H1D,H1E), C2(H2A,H2B), C3(H3A,H3B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C11(H11A,H11B),
 C10(H10A,H10B)
7.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E), N4(H4C,H4D,H4E)
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_shelx_res_checksum              70760
_shelx_hkl_checksum              74381
_olex2_submission_special_instructions 'No special instructions were received'