New lead-iodide formates with a strong second-harmonic generation response and suitable birefringence obtained by the substitution strategy.
Zhang, Xiang-Yu; Zhou, Zi-Qi; Bao, Wen-Xiu; Tang, Hong-Xin; Fu, Rui-Biao; Ma, Zu-Ju; Wu, Xin-Tao; Chemical science 14 (2022) 136–142; doi:10.1039/d2sc05216d

data_1567998
_publ_section_title
;
 New lead-iodide formates with a strong second-harmonic generation
 response and suitable birefringence obtained by the substitution
 strategy.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              136
_journal_page_last               142
_journal_paper_doi               10.1039/d2sc05216d
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C2 H2 I2 K2 O4 Pb'
_chemical_formula_sum            'C2 H2 I2 K2 O4 Pb'
_chemical_formula_weight         629.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           38
_space_group_name_Hall           'A 2 -2'
_space_group_name_H-M_alt        'A m m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2ck8nw
_audit_creation_date             2022-03-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-07-19 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.80240(10)
_cell_length_b                   6.7740(2)
_cell_length_c                   13.6260(4)
_cell_measurement_reflns_used    2209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.3390
_cell_measurement_theta_min      5.6340
_cell_volume                     535.58(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      6.00  58.00   0.50    0.11    --   73.53 -38.00  90.00  104
  2  \w      1.00  67.00   0.50    0.11    --   73.53 -38.00 120.00  132
  3  \w    100.00 145.00   0.50    0.11    --   73.53  19.00 -60.00   90
  4  \w     64.00  90.00   0.50    0.11    --   73.53  19.00 -60.00   52
  5  \w      0.00  70.00   0.50    0.11    --   73.53 -38.00 -30.00  140
  6  \w     44.00  91.00   0.50    0.11    --   73.53 -99.00  30.00   94
  7  \w     28.00 109.00   0.50    0.11    --   73.53-125.00   0.00  162
  8  \w     13.00  39.00   0.50    0.11    --   73.53 -99.00  30.00   52
  9  \w     74.00 111.00   0.50    0.11    --   73.53-125.00-120.00   74
 10  \w     69.00  99.00   0.50    0.11    --   73.53-125.00-180.00   60
 11  \w     22.00  55.00   0.50    0.11    --   73.53-125.00-120.00   66
 12  \w     26.00  72.00   0.50    0.05    --   -0.62  19.00 -30.00   92
 13  \w    -68.00 -16.00   0.50    0.11    --  -74.78  77.00 -90.00  104
 14  \w    -98.00 -71.00   0.50    0.11    --  -74.78  77.00 -90.00   54
 15  \w    -11.00  14.00   0.50    0.05    --   -0.62 -38.00-180.00   50
 16  \w    -57.00 -29.00   0.50    0.05    --   -0.62 -38.00-180.00   56
 17  \w   -122.00 -95.00   0.50    0.11    --  -74.78 -99.00-150.00   54
 18  \w   -146.00 -56.00   0.50    0.11    --  -74.78 -77.00  90.00  180
 19  \w   -145.00 -99.00   0.50    0.11    --  -74.78 -99.00 120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1186789000
_diffrn_orient_matrix_UB_12      0.1592996000
_diffrn_orient_matrix_UB_13      -0.0288324000
_diffrn_orient_matrix_UB_21      -0.1881489000
_diffrn_orient_matrix_UB_22      -0.0697230000
_diffrn_orient_matrix_UB_23      0.0451581000
_diffrn_orient_matrix_UB_31      0.0615817000
_diffrn_orient_matrix_UB_32      0.0939801000
_diffrn_orient_matrix_UB_33      0.0824080000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2119
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        52.036
_diffrn_reflns_theta_max         52.036
_diffrn_reflns_theta_min         5.646
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    56.272
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.98a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    3.902
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 186 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.00054(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         473
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0193
_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^)+(0.0276P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0465
_reflns_Friedel_coverage         0.648
_reflns_Friedel_fraction_full    0.707
_reflns_Friedel_fraction_max     0.707
_reflns_number_gt                473
_reflns_number_total             473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05216d2.cif
_cod_data_source_block           zxy_147_11_autored
_cod_depositor_comments
'Adding full bibliography for 1567997--1567998.cif.'
_cod_database_code               1567998
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_shelx_res_checksum              66339
_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 2.339
_oxdiff_exptl_absorpt_empirical_full_min 0.487