Jahn-Teller Effect on Framework Flexibility of Hybrid Organic-Inorganic Perovskites.
Gui, Di; Ji, Lijun; Muhammad, Azeem; Li, Wei; Cai, Weizhao; Li, Yanchun; Li, Xiaodong; Wu, Xiang; Lu, Peixiang; The journal of physical chemistry letters  (2018) 751–755; doi:10.1021/acs.jpclett.7b03229

data_8000275
_publ_section_title
;
 Jahn-Teller Effect on Framework Flexibility of Hybrid Organic-Inorganic
 Perovskites.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              751
_journal_page_last               755
_journal_paper_doi               10.1021/acs.jpclett.7b03229
_journal_year                    2018
_chemical_formula_moiety         '0.25(C12 H12 O24 Zn4), C H6 N3'
_chemical_formula_sum            'C4 H9 N3 O6 Zn'
_chemical_formula_weight         260.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3010(3)
_cell_length_b                   11.6888(5)
_cell_length_c                   8.9533(4)
_cell_measurement_reflns_used    13670
_cell_measurement_temperature    120.12(19)
_cell_measurement_theta_max      30.3730
_cell_measurement_theta_min      3.7910
_cell_volume                     868.73(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.12(19)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9934
_diffrn_measured_fraction_theta_max 0.9543
_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     11.00  74.00   0.50    0.50    --   -0.70  57.00 150.00  126
  2  \w     15.00  76.00   0.50    0.50    --   -0.70  57.00 -60.00  122
  3  \w    -26.00  75.00   0.50    0.50    --   -0.70  57.00   0.00  202
  4  \w    -26.00  53.00   0.50    0.50    --   -0.70  57.00 120.00  158
  5  \w    -26.00   5.00   0.50    0.50    --   -0.70  57.00 150.00   62
  6  \w    -26.00  80.00   0.50    0.50    --   -0.70  57.00  60.00  212
  7  \w    -26.00  68.00   0.50    0.50    --   -0.70  57.00-150.00  188
  8  \w    -25.00  63.00   0.50    0.50    --   -0.70  57.00 -90.00  176
  9  \w    -26.00   0.00   0.50    0.50    --   -0.70  57.00 -60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0505567000
_diffrn_orient_matrix_UB_12      0.0325080000
_diffrn_orient_matrix_UB_13      -0.0477284000
_diffrn_orient_matrix_UB_21      0.0402905000
_diffrn_orient_matrix_UB_22      0.0506885000
_diffrn_orient_matrix_UB_23      0.0223029000
_diffrn_orient_matrix_UB_31      0.0559144000
_diffrn_orient_matrix_UB_32      -0.0071399000
_diffrn_orient_matrix_UB_33      -0.0592138000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0084
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21706
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         30.31
_diffrn_reflns_theta_min         3.77
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.211
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0633P)^2^+0.5329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                1229
_reflns_number_total             1252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Zn-120K.cif
_cod_data_source_block           Zn_120_00-multiscan
_cod_database_code               8000275
_chemical_oxdiff_formula         'C4 H9 O3 N4 Zn1'
_reflns_odcompleteness_completeness 99.34
_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,H) groups
2. Others
 Fixed Sof: H2A(0.5) H2B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
3.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.204
_oxdiff_exptl_absorpt_empirical_full_min 0.862