Constructing moisture-stable hybrid lead iodine semiconductors based on hydrogen-bond-free and dual-iodine strategies
Liu, Guang-Ning; Zhao, Ruo-Yu; Xu, Rang-Dong; Liu, Qisheng; Xu, Bo; Wang, Yang-Yang; Wu, Qian; Wang, Jun-Nuan; Nie, Yong; Li, Cuncheng; Journal of Materials Chemistry C 7 (2019) 7700–; doi:10.1039/C9TC01967G

data_7237852
_publ_section_title
;
 Constructing moisture-stable hybrid lead iodine semiconductors based on
 hydrogen-bond-free and dual-iodine strategies
;
_journal_issue                   25
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              7700
_journal_paper_doi               10.1039/C9TC01967G
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'I6 Pb2, C48 H32 Cl1.29 I0.71 Mn2 N8'
_chemical_formula_sum            'C48 H32 Cl1.29 I6.71 Mn2 N8 Pb2'
_chemical_formula_weight         2142.30
_chemical_name_systematic        '[Mn(1,10-Phenanthroline)2Cl0.65I0.35]2Pb2I6'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-02-11 deposited with the CCDC.	2019-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                71.256(5)
_cell_angle_beta                 77.764(4)
_cell_angle_gamma                68.460(5)
_cell_formula_units_Z            2
_cell_length_a                   12.0083(6)
_cell_length_b                   15.9672(8)
_cell_length_c                   16.8500(9)
_cell_measurement_reflns_used    12886
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9820
_cell_measurement_theta_min      3.4950
_cell_volume                     2829.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -11.00   83.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -       15.7007   77.0000  -60.0000 94

  2 omega  -52.00   42.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -77.0000 -180.0000 94

  3 omega   -1.00   83.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -       15.7007   57.0000   60.0000 84

  4 omega   -3.00   85.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -       15.7007   37.0000  120.0000 88

  5 omega  -64.00   -8.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -      -16.8725  113.0000   36.5546 56

  6 omega  -52.00    9.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -57.0000   60.0000 61

  7 omega  -54.00   35.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -37.0000  -60.0000 89

  8 omega   35.00   88.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -       15.7007  178.0000 -180.0000 53

  9 omega  -66.00  -12.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -      -16.8725  117.0000 -106.5542 54

 10 omega  -23.00   23.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -      -16.8725 -101.0000   86.0000 46

 11 omega  -84.00    0.00   1.0000   25.4500
omega____ theta____ kappa____ phi______ frames
    -      -16.8725  -57.0000 -180.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0415518000
_diffrn_orient_matrix_UB_12      -0.0167514000
_diffrn_orient_matrix_UB_13      0.0320507000
_diffrn_orient_matrix_UB_21      -0.0172190000
_diffrn_orient_matrix_UB_22      -0.0157781000
_diffrn_orient_matrix_UB_23      -0.0288985000
_diffrn_orient_matrix_UB_31      0.0453420000
_diffrn_orient_matrix_UB_32      -0.0439041000
_diffrn_orient_matrix_UB_33      0.0116797000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43227
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.253
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_description       block
_exptl_crystal_F_000             1935
_exptl_crystal_preparation       'photoconductive property'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.545
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         10505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+17.6771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8771
_reflns_number_total             10505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9tc01967g2.cif
_cod_data_source_block           MnPhen-Pb2I6
_cod_original_cell_volume        2829.6(3)
_cod_database_code               7237852
_chemical_oxdiff_formula         'C H N O Mn I Pb'
_shelx_estimated_absorpt_t_max   'not measured'
_shelx_estimated_absorpt_t_min   'not measured'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(I7) = Uanis(Cl1)
Uanis(I8) = Uanis(Cl2)
3. Others
 Sof(Cl1)=Sof(Cl2)=1-FVAR(1)
 Sof(I7)=Sof(I8)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              81719
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'