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_1569698
_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         'C4 H11 Cd I3 N2'
_chemical_formula_sum            'C4 H11 Cd I3 N2'
_chemical_formula_weight         580.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 121.298(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3680(6)
_cell_length_b                   7.13490(10)
_cell_length_c                   13.7778(5)
_cell_measurement_reflns_used    4517
_cell_measurement_temperature    109(3)
_cell_measurement_theta_max      77.6930
_cell_measurement_theta_min      3.7300
_cell_volume                     1206.88(9)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.963
_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    -20.00  24.00   0.50    0.05    --  -45.86  19.00-180.00   88
  2  \w    -22.00  26.00   0.50    0.05    --  -45.86  19.00   0.00   96
  3  \w   -102.00 -77.00   0.50    0.05    -- -104.50 112.00  46.00   50
  4  \w    -75.00 -13.00   0.50    0.05    --  -45.86 112.00  46.00  124
  5  \w     40.00  94.00   0.50    0.05    --  108.75-125.00 120.00  108
  6  \w     52.00  78.00   0.50    0.05    --  108.75 -95.00  90.00   52
  7  \w     86.00 111.00   0.50    0.05    --  108.75-125.00  30.00   50
  8  \w     86.00 112.00   0.50    0.05    --  108.75-125.00   0.00   52
  9  \w     67.00  93.00   0.50    0.05    --  108.75-112.00 -46.00   52
 10  \w     10.00  53.00   0.50    0.05    --   45.86-112.00 -46.00   86
 11  \w     86.00 111.00   0.50    0.05    --  108.75 -86.00 -54.91   50
 12  \w     39.00  70.00   0.50    0.05    --  108.75 -95.00 -30.00   62
 13  \w     36.00  72.00   0.50    0.05    --  108.75 -95.00   0.00   72
 14  \w     79.00 104.00   0.50    0.05    --  108.75 -95.00   0.00   50
 15  \w     39.00  73.00   0.50    0.05    --  108.75 -61.00  30.00   68
 16  \w     39.00  73.00   0.50    0.05    --  108.75 -61.00 120.00   68
 17  \w     78.00 105.00   0.50    0.05    --  108.75 -76.00 -52.94   54
 18  \w     42.00  67.00   0.50    0.05    --  108.75 -61.00   0.00   50
 19  \w     40.00  71.00   0.50    0.05    --  108.75 -61.00 -60.00   62
 20  \w     37.00  72.00   0.50    0.05    --  108.75 -61.00-120.00   70
 21  \w     38.00  70.00   0.50    0.05    --  108.75 -77.00-150.00   64
 22  \w     81.00 106.00   0.50    0.05    --  108.75 -77.00-150.00   50
 23  \w    133.00 158.00   0.50    0.05    --  108.75  15.00-180.00   50
 24  \w    128.00 177.00   0.50    0.05    --  108.75  45.00-150.00   98
 25  \w     91.00 149.00   0.50    0.05    --  108.75  61.00-180.00  116
 26  \w     96.00 126.00   0.50    0.05    --  108.75  15.00-180.00   60
 27  \w    101.00 127.00   0.50    0.05    --  108.75  61.00-120.00   52
 28  \w    130.00 155.00   0.50    0.05    --  108.75  61.00-120.00   50
 29  \w    100.00 129.00   0.50    0.05    --  108.75  30.00  30.00   58
 30  \w    119.00 169.00   0.50    0.05    --  108.75 125.00 150.00  100
 31  \w    109.00 135.00   0.50    0.05    --  108.75 112.00  46.00   52
 32  \w     84.00 132.00   0.50    0.05    --  108.75 125.00-120.00   96
 33  \w    150.00 177.00   0.50    0.05    --  108.75 125.00-120.00   54
 34  \w    -54.00 -28.00   0.50    0.05    --  -45.86 -77.00-120.00   52
 35  \w   -112.00 -58.00   0.50    0.05    --  -45.86 -77.00-120.00  108
 36  \w   -122.00 -83.00   0.50    0.05    -- -104.50-112.00 -46.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1124937000
_diffrn_orient_matrix_UB_12      0.0344454000
_diffrn_orient_matrix_UB_13      -0.0147218000
_diffrn_orient_matrix_UB_21      0.0523365000
_diffrn_orient_matrix_UB_22      0.1338262000
_diffrn_orient_matrix_UB_23      0.1027230000
_diffrn_orient_matrix_UB_31      -0.0188778000
_diffrn_orient_matrix_UB_32      0.1658857000
_diffrn_orient_matrix_UB_33      -0.0797592000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4712
_diffrn_reflns_point_group_measured_fraction_full 0.827
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.071
_diffrn_reflns_theta_min         7.179
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    74.345
_exptl_absorpt_correction_T_max  0.256
_exptl_absorpt_correction_T_min  0.030
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    3.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.465
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.281
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2046
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0874P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    0.677
_reflns_Friedel_fraction_max     0.624
_reflns_number_gt                2036
_reflns_number_total             2046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03052k5.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 1569697--1569698.cif.'
_cod_database_code               1569698
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4N2H11CdI3
_shelx_estimated_absorpt_t_max   0.057
_shelx_estimated_absorpt_t_min   0.022
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.01(2)
 -0.01(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
3.a Ternary CH refined with riding coordinates:
 N2(H2)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C4(H4A,H4B), C1(H1C,H1D), C3(H3A,H3B), C2(H2A,H2B)
;
_shelx_res_checksum              57132
_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 1.693
_oxdiff_exptl_absorpt_empirical_full_min 0.544