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_7709965
_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_absolute_configuration rm
_chemical_formula_moiety         'I3 Pb0.5, C5 H14 N2'
_chemical_formula_sum            'C6 H14 I3 N Pb0.5'
_chemical_formula_weight         584.48
_chemical_name_systematic        S-2-I
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6367(3)
_cell_length_b                   10.2416(3)
_cell_length_c                   8.7513(2)
_cell_measurement_reflns_used    9600
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.8740
_cell_measurement_theta_min      3.9530
_cell_volume                     1311.85(6)
_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    'ShelXT (Sheldrick, 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 0.958
_diffrn_measured_fraction_theta_max 0.962
_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     12.00  40.00   0.50    0.50    --   -0.30  32.00  43.00   56
  2  \w    -33.00  29.00   0.50    0.50    --   -0.30 -82.00 -90.00  124
  3  \w    -44.00  24.00   0.50    0.50    --   -0.30 -77.00  30.00  136
  4  \w    -31.00  39.00   0.50    0.50    --   -0.30  77.00 120.00  140
  5  \w     48.00  75.00   0.50    0.50    --   -0.30  32.00  43.00   54
;
_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      -0.0158956000
_diffrn_orient_matrix_UB_12      0.0348109000
_diffrn_orient_matrix_UB_13      -0.0648295000
_diffrn_orient_matrix_UB_21      0.0117265000
_diffrn_orient_matrix_UB_22      0.0597834000
_diffrn_orient_matrix_UB_23      0.0359138000
_diffrn_orient_matrix_UB_31      0.0442478000
_diffrn_orient_matrix_UB_32      -0.0032476000
_diffrn_orient_matrix_UB_33      -0.0328294000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11961
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.629
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    13.489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37516
_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    2.959
_exptl_crystal_description       prism
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.814
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Flack x determined using 1111 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0103P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0400
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.914
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                2794
_reflns_number_total             2850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00557c2.cif
_cod_data_source_block           s-2-i
_cod_original_formula_sum        'C6 H14 I3 N Pb0.50'
_cod_database_code               7709965
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.057
_reflns_odcompleteness_completeness 99.35
_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
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C4(H4A,H4B), C2(H2C,H2D), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              1411
_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 1.571
_oxdiff_exptl_absorpt_empirical_full_min 0.714