Facile Synthesis of 1D Organic‒Inorganic Perovskite Micro-Belts with High Water Stability for Sensor and Photonic Applications
Yang, Xiao-Gang; Ma, Lufang; Yan, Dongpeng; Chemical Science  (2019) –; doi:10.1039/C9SC00162J

data_1550725
_publ_section_title
;
 Facile Synthesis of 1D Organic--Inorganic Perovskite Micro-Belts with
 High Water Stability for Sensor and Photonic Applications
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00162J
_journal_year                    2019
_chemical_formula_moiety         'Cl2 Pb, 0.5(Cl), C6 H5 N'
_chemical_formula_sum            'C6 H5 Cl2.5 N Pb'
_chemical_formula_weight         386.96
_chemical_name_systematic        OIP-AD
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-19 deposited with the CCDC.    2019-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                100.672(6)
_cell_angle_beta                 91.860(6)
_cell_angle_gamma                102.273(6)
_cell_formula_units_Z            2
_cell_length_a                   4.0291(3)
_cell_length_b                   8.8371(6)
_cell_length_c                   12.3963(10)
_cell_measurement_reflns_used    1530
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.7420
_cell_measurement_theta_min      4.7600
_cell_volume                     422.64(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.9974
_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    -16.00  82.00   1.00    2.06    --   12.45  57.00  60.00   98
  2  \w    -20.00  15.00   1.00    2.06    --   12.45  77.00 -60.00   35
  3  \w    -55.00  33.00   1.00    2.06    --   12.45 -57.00 -90.00   88
  4  \w    -18.00  47.00   1.00    2.06    --   12.45 -99.00-180.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0797290000
_diffrn_orient_matrix_UB_12      -0.0682044000
_diffrn_orient_matrix_UB_13      -0.0393578000
_diffrn_orient_matrix_UB_21      -0.0526119000
_diffrn_orient_matrix_UB_22      -0.0402638000
_diffrn_orient_matrix_UB_23      0.0431277000
_diffrn_orient_matrix_UB_31      -0.1533509000
_diffrn_orient_matrix_UB_32      0.0273082000
_diffrn_orient_matrix_UB_33      0.0005211000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.1073
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3273
_diffrn_reflns_theta_full        25.4984
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.35
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.0404
_exptl_crystal_description       block
_exptl_crystal_F_000             339.9181
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.5972
_refine_diff_density_min         -2.4223
_refine_diff_density_rms         0.4122
_refine_ls_d_res_high            0.8255
_refine_ls_d_res_low             6.0739
_refine_ls_goodness_of_fit_ref   0.9427
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    10
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1560
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.9408
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              4
_reflns_limit_h_min              -4
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                1357
_reflns_number_total             1560
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9sc00162j2.cif
_cod_data_source_block           20160719e
_cod_original_cell_volume        422.64(5)
_cod_database_code               1550725
_chemical_oxdiff_formula         'C1 H1 N1 Cl1 Pb1'
_chemical_oxdiff_usercomment     Y567
_reflns_odcompleteness_completeness 99.77
_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 N(H) groups
2. Rigid bond restraints
 C5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1a), C2(H2), C5(H5), C6(H6)
;
_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 2.854
_oxdiff_exptl_absorpt_empirical_full_min 0.589