Methylpiperazine Based 0D Chiral Hybrid Lead Halides for Second Harmonic Generation
Jia, Xiaodi; Zheng, Yongshen; Cheng, Puxin; Han, Xiao; Xu, Liang; Xu, Jialiang; Dalton Transactions  (2022) –; doi:10.1039/D2DT00557C

data_7709967
_publ_section_title
;
 Methylpiperazine Based 0D Chiral Hybrid Lead Halides for Second Harmonic
 Generation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00557C
_journal_year                    2022
_chemical_formula_moiety         'I3 Pb0.5, C5 H14 N2, 1.5(H2 O)'
_chemical_formula_sum            'C5 H14 I3 N3.5 O0.25 Pb0.5'
_chemical_formula_weight         611.49
_chemical_name_systematic        rac-2-I
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-27 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.420(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5613(2)
_cell_length_b                   10.0810(2)
_cell_length_c                   15.1805(3)
_cell_measurement_reflns_used    19520
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      31.1920
_cell_measurement_theta_min      4.2530
_cell_volume                     1403.53(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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      7.00  32.00   0.50    0.50    --   -0.30  58.00 -30.00   50
  2  \w    -59.00 -32.00   0.50    0.50    --   -0.30 -58.00-171.00   54
  3  \w    -32.00  47.00   0.50    0.50    --   -0.30  77.00-180.00  158
  4  \w    -32.00  48.00   0.50    0.50    --   -0.30  77.00  60.00  160
  5  \w    -49.00  31.00   0.50    0.50    --   -0.30 -77.00 -90.00  160
  6  \w     -2.00  32.00   0.50    0.50    --   -0.30  38.00  90.00   68
  7  \w     39.00  65.00   0.50    0.50    --   -0.30  38.00  90.00   52
  8  \w    -86.00  18.00   0.50    0.50    --   -0.30 -38.00-150.00  208
  9  \w    -24.00  44.00   0.50    0.50    --   -0.30  77.00  30.00  136
 10  \w      5.00  30.00   0.50    0.50    --   -0.30  38.00-180.00   50
 11  \w    -11.00  32.00   0.50    0.50    --   -0.30  77.00-120.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0464195000
_diffrn_orient_matrix_UB_12      0.0092268000
_diffrn_orient_matrix_UB_13      -0.0451329000
_diffrn_orient_matrix_UB_21      -0.0408033000
_diffrn_orient_matrix_UB_22      0.0476738000
_diffrn_orient_matrix_UB_23      0.0167000000
_diffrn_orient_matrix_UB_31      0.0465050000
_diffrn_orient_matrix_UB_32      0.0509135000
_diffrn_orient_matrix_UB_33      -0.0075106000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23779
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         3.569
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    12.620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.894
_exptl_crystal_description       plate
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.532
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2467
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+2.3039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2403
_reflns_number_total             2467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00557c2.cif
_cod_data_source_block           rac-2-i
_cod_original_formula_sum        'C5 H14 I3 N3.50 O0.25 Pb0.50'
_cod_database_code               7709967
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.187
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H3D-H1B
 2.1 with sigma of 0.02
 H3D-H4D
 2.1 with sigma of 0.02
 H1B-H3C
 2.1 with sigma of 0.02
 H1B-H3D
 2.1 with sigma of 0.02
3. Others
 Fixed Sof: H4C(0.5) H4D(0.5)
4.a Free rotating group:
 O4(H4C,H4D), O3(H3C,H3D)
4.b Ternary CH refined with riding coordinates:
 C1(H1)
4.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C2(H2C,H2D)
4.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              84005
_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 1.640
_oxdiff_exptl_absorpt_empirical_full_min 0.760