From H<sub>12</sub>C<sub>4</sub>N<sub>2</sub>CdI<sub>4</sub> to H<sub>11</sub>C<sub>4</sub>N<sub>2</sub>CdI<sub>3</sub>: a highly polarizable CdNI<sub>3</sub> tetrahedron induced a sharp enhancement of second harmonic generation response and birefringence.
Wu, Huai-Yu; Hu, Chun-Li; Xu, Miao-Bin; Chen, Qian-Qian; Ma, Nan; Huang, Xiao-Ying; Du, Ke-Zhao; Chen, Jin; Chemical science 14 (2023) 9533–9542; doi:10.1039/d3sc03052k

data_1569697
_publ_section_title
;
 From H<sub>12</sub>C<sub>4</sub>N<sub>2</sub>CdI<sub>4</sub> to
 H<sub>11</sub>C<sub>4</sub>N<sub>2</sub>CdI<sub>3</sub>: a highly
 polarizable CdNI<sub>3</sub> tetrahedron induced a sharp enhancement of
 second harmonic generation response and birefringence.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              9533
_journal_page_last               9542
_journal_paper_doi               10.1039/d3sc03052k
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'Cd I4, C4 H12 N2'
_chemical_formula_sum            'C4 H12 Cd I4 N2'
_chemical_formula_weight         708.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-19 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0318(5)
_cell_length_b                   12.2358(6)
_cell_length_c                   13.0518(7)
_cell_measurement_reflns_used    4947
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5740
_cell_measurement_theta_min      3.6720
_cell_volume                     1442.37(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (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                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_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    -43.00  18.00   1.00    1.00    --   15.65 -57.00 -90.00   61
  2  \w    -21.00  39.00   1.00    1.00    --   15.65 -19.00 -90.00   60
  3  \w    -25.00  21.00   1.00    1.00    --  -16.59 -99.00 -90.00   46
  4  \w    -24.00  14.00   1.00    1.00    --  -16.59 -99.00-180.00   38
  5  \w     36.00  61.00   1.00    1.00    --   15.65-178.00 -60.00   25
  6  \w    -19.00   8.00   1.00    1.00    --  -16.59 -99.00  90.00   27
  7  \w     -1.00  85.00   1.00    1.00    --   15.65  38.00  90.00   86
  8  \w     49.00  88.00   1.00    1.00    --   15.65 178.00-120.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0258701000
_diffrn_orient_matrix_UB_12      -0.0532843000
_diffrn_orient_matrix_UB_13      -0.0115237000
_diffrn_orient_matrix_UB_21      -0.0181187000
_diffrn_orient_matrix_UB_22      -0.0081083000
_diffrn_orient_matrix_UB_23      0.0523735000
_diffrn_orient_matrix_UB_31      -0.0718830000
_diffrn_orient_matrix_UB_32      0.0213023000
_diffrn_orient_matrix_UB_33      -0.0089695000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10982
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.538
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.037
_exptl_absorpt_correction_T_max  0.109
_exptl_absorpt_correction_T_min  0.023
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.86
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.264
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.222
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(12)
_refine_ls_extinction_coef       0.0139(5)
_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   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0381P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                2643
_reflns_number_total             2902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03052k5.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 1569697--1569698.cif.'
_cod_database_code               1569697
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         (H12C4N2)CdI4
_shelx_estimated_absorpt_t_max   0.132
_shelx_estimated_absorpt_t_min   0.042
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(12)
 0.45(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C1(H1C,H1D), C2(H2C,H2D), C4(H4A,H4B), C3(H3A,H3B)
;
_shelx_res_checksum              88848
_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 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.699