2(C<sub>3</sub>H<sub>7</sub>N<sub>6</sub>)<sup>+</sup>·2Cl<sup>-</sup>·H<sub>2</sub>O: an ultraviolet nonlinear optical crystal with large birefrigence and strong second-harmonic generation.
Liu, Lehui; Hu, Chun-Li; Bai, Zhiyong; Yuan, Feifei; Huang, Yisheng; Zhang, Lizhen; Lin, Zhoubin; Chemical communications (Cambridge, England) 56 (2020) 14657–14660; doi:10.1039/d0cc06558g

data_7127719
_publ_section_title
;
 2(C<sub>3</sub>H<sub>7</sub>N<sub>6</sub>)<sup>+</sup>&#x00B7;2Cl<sup>-</sup>&#x00B7;H<sub>2</sub>O:
 an ultraviolet nonlinear optical crystal with large birefrigence and
 strong second-harmonic generation.
;
_journal_issue                   93
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14657
_journal_page_last               14660
_journal_paper_doi               10.1039/d0cc06558g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(Cl), 2(C3 H7 N6), 0.5(H4 O2)'
_chemical_formula_sum            'C6 H16 Cl2 N12 O'
_chemical_formula_weight         343.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7812(5)
_cell_length_b                   12.2467(4)
_cell_length_c                   6.9816(2)
_cell_measurement_reflns_used    3929
_cell_measurement_temperature    300.00(11)
_cell_measurement_theta_max      60.2170
_cell_measurement_theta_min      4.5990
_cell_volume                     1434.82(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_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      air
_diffrn_ambient_temperature      300.00(11)
_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 0.992
_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     38.00  64.00   0.50    0.05    --   -1.56  19.00-180.00   52
  2  \w    -19.00   7.00   0.50    0.05    --   -1.56 -38.00   0.00   52
  3  \w    -12.00  28.00   0.50    0.05    --   -1.56  19.00-180.00   80
  4  \w    -75.00 -22.00   0.50    0.05    --   -1.56 -38.00   0.00  106
  5  \w     -3.00  23.00   0.50    0.08    --   72.34 -19.00 -60.00   52
  6  \w     23.00  60.00   0.50    0.08    --   72.34-125.00 -60.00   74
  7  \w     -2.00  24.00   0.50    0.08    --   72.34 -19.00   0.00   52
  8  \w     49.00 127.00   0.50    0.08    --   72.34  77.00 -90.00  156
  9  \w     86.00 144.00   0.50    0.08    --   72.34 125.00   0.00  116
 10  \w     42.00 102.00   0.50    0.08    --   72.34 -99.00 -30.00  120
 11  \w     39.00  65.00   0.50    0.08    --   72.34 -57.00 -90.00   52
 12  \w     64.00 111.00   0.50    0.08    --   72.34-125.00 -60.00   94
 13  \w    -96.00 -68.00   0.50    0.08    --  -75.46  77.00  90.00   56
 14  \w    -25.00   0.00   0.50    0.08    --  -75.46  19.00-120.00   50
 15  \w   -111.00 -80.00   0.50    0.08    --  -75.46-125.00  30.00   62
 16  \w    -60.00 -21.00   0.50    0.08    --  -75.46  57.00-150.00   78
 17  \w    -40.00 -14.00   0.50    0.08    --  -75.46  38.00  30.00   52
 18  \w    -51.00 -23.00   0.50    0.08    --  -75.46 125.00 120.00   56
 19  \w   -109.00 -68.00   0.50    0.08    --  -75.46 125.00 120.00   82
 20  \w    -62.00  -2.00   0.50    0.08    --  -75.46  57.00  90.00  120
 21  \w    -58.00 -12.00   0.50    0.08    --  -75.46  57.00  30.00   92
 22  \w   -142.00-116.00   0.50    0.08    --  -75.46-125.00  30.00   52
 23  \w    -37.00 -10.00   0.50    0.08    --  -75.46  38.00 -30.00   54
 24  \w    -65.00 -11.00   0.50    0.08    --  -75.46  77.00  90.00  108
 25  \w    -58.00  -7.00   0.50    0.08    --  -75.46  57.00 150.00  102
 26  \w   -137.00 -95.00   0.50    0.08    --  -75.46 -99.00  90.00   84
;
_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      -0.0270370000
_diffrn_orient_matrix_UB_12      -0.0884917000
_diffrn_orient_matrix_UB_13      -0.0918658000
_diffrn_orient_matrix_UB_21      0.0726913000
_diffrn_orient_matrix_UB_22      -0.0171328000
_diffrn_orient_matrix_UB_23      -0.0729445000
_diffrn_orient_matrix_UB_31      0.0185403000
_diffrn_orient_matrix_UB_32      -0.0619551000
_diffrn_orient_matrix_UB_33      0.1519099000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7725
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.643
_diffrn_reflns_theta_min         3.885
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    2.795
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
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    1.589
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 396 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1523
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0469P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.650
_reflns_Friedel_fraction_full    0.798
_reflns_Friedel_fraction_max     0.764
_reflns_number_gt                1288
_reflns_number_total             1523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06558g2.cif
_cod_data_source_block           melcl
_cod_database_code               7127719
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C NO Cl'
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.488
_diffrn_oxdiff_digest_frames
;
017fef63c6393b89775bef17ec276c68ef02054adf8
;
_diffrn_oxdiff_digest_hkl
;
01c6b4af435afb28772c3f8b1da35798ab510e
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5)
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Aromatic/amide H refined with riding coordinates:
 N5(H5)
;
_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 3.372
_oxdiff_exptl_absorpt_empirical_full_min 0.306