A new solvate of clonixin and a comparison of the two clonixin solvates
Zhoujin, Yunping; Zhang, Mingtao; Parkin, Sean; Li, Tonglei; Yu, Faquan; Long, Sihui; RSC Advances 11 (2021) 24836–24842; doi:10.1039/D1RA03623H

data_7243237
_publ_section_title
;
 A new solvate of clonixin and a comparison of the two clonixin solvates
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              24836
_journal_page_last               24842
_journal_paper_doi               10.1039/D1RA03623H
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C13 H11 Cl N2 O2, C4 H9 N O'
_chemical_formula_sum            'C17 H20 Cl N3 O3'
_chemical_formula_weight         349.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2021-04-25 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.548(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4376(4)
_cell_length_b                   5.92226(13)
_cell_length_c                   19.0732(6)
_cell_measurement_reflns_used    4210
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.9240
_cell_measurement_theta_min      4.6980
_cell_volume                     1714.31(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4674
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.995
_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     26.00 103.00   1.00    1.00    --   42.20  38.00 -60.00   77
  2  \w     26.00 114.00   1.00    1.00    --   42.20  38.00-150.00   88
  3  \w     16.00  64.00   1.00    2.99    --   92.50 -77.00 150.00   48
  4  \w     81.00 107.00   1.00    2.99    --   92.50 -61.00 -60.00   26
  5  \w     93.00 165.00   1.00    2.99    --   92.50  45.00  90.00   72
  6  \w     12.00  48.00   1.00    2.99    --   92.50 -95.00  30.00   36
  7  \w     19.00  96.00   1.00    2.99    --   92.50 -45.00 150.00   77
  8  \w    121.00 157.00   1.00    2.99    --   92.50  15.00 -30.00   36
  9  \w     10.00  53.00   1.00    2.99    --   92.50 -95.00   0.00   43
 10  \w     59.00  84.00   1.00    2.99    --   92.50 -95.00   0.00   25
 11  \w     93.00 127.00   1.00    2.99    --   92.50  61.00  30.00   34
 12  \w     46.00  72.00   1.00    2.99    --   92.50 -61.00 -60.00   26
 13  \w     18.00  44.00   1.00    2.99    --   92.50 -30.00-180.00   26
 14  \w     41.00 103.00   1.00    2.99    --   92.50  15.00 -30.00   62
 15  \w     89.00 115.00   1.00    2.99    --   92.50 -90.00 123.15   26
 16  \w     81.00 107.00   1.00    2.99    --   92.50 125.00   0.00   26
 17  \w    130.00 156.00   1.00    2.99    --   92.50 125.00   0.00   26
 18  \w     73.00  99.00   1.00    2.99    --   92.50  45.00-150.00   26
 19  \w     39.00  72.00   1.00    2.99    --   92.50 -95.00 150.00   33
 20  \w     24.00  49.00   1.00    2.99    --   92.50-125.00-180.00   25
 21  \w     40.00  75.00   1.00    2.99    --   92.50 -90.00 123.15   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0904347000
_diffrn_orient_matrix_UB_12      -0.0916939000
_diffrn_orient_matrix_UB_13      0.0097124000
_diffrn_orient_matrix_UB_21      0.0347221000
_diffrn_orient_matrix_UB_22      -0.0278531000
_diffrn_orient_matrix_UB_23      0.0805398000
_diffrn_orient_matrix_UB_31      -0.0303038000
_diffrn_orient_matrix_UB_32      0.2418509000
_diffrn_orient_matrix_UB_33      0.0129925000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9510
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.856
_diffrn_reflns_theta_min         4.717
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_F_000             736
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0610P)^2^+0.4319P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2517
_reflns_number_total             3017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03623h2.cif
_cod_data_source_block           17228-e
_cod_database_code               7243237
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cl1'
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N7(H7), C4(H4), C12(H12), C11(H11), C2(H2), C13(H13), C3(H3)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C)
2.c Idealised tetrahedral OH refined as rotating group:
 O16(H16)
;
_olex2_date_sample_data_collection 2017-03-08
_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 1.299
_oxdiff_exptl_absorpt_empirical_full_min 0.812