Structure and Morphology of Indole Analogue Crystals.
Pisarek, Joanna; Malinska, Maura; ACS omega 5 (2020) 17141–17151; doi:10.1021/acsomega.0c01020

data_4517845
_publ_section_title
;
 Structure and Morphology of Indole Analogue Crystals.
;
_journal_issue                   28
_journal_name_full               'ACS omega'
_journal_page_first              17141
_journal_page_last               17151
_journal_paper_doi               10.1021/acsomega.0c01020
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C8 H6 N2 O2'
_chemical_formula_sum            'C8 H6 N2 O2'
_chemical_formula_weight         162.15
_chemical_name_systematic        5-Nitroindole
_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             2019-08-02
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.730(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.75839(9)
_cell_length_b                   12.0667(3)
_cell_length_c                   15.8045(4)
_cell_measurement_reflns_used    7708
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.3100
_cell_measurement_theta_min      2.5580
_cell_volume                     716.70(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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     49.00  99.00   1.00   50.00    --   27.00 160.00  90.00   50
  2  \w    -17.00 100.00   1.00   50.00    --   27.00  19.00 120.00  117
  3  \w      6.00  96.00   1.00   50.00    --   27.00  57.00 -30.00   90
  4  \w     49.00  99.00   1.00   50.00    --   27.00 160.00  30.00   50
  5  \w    -42.00  47.00   1.00   50.00    --   27.00 -57.00  90.00   89
  6  \w      6.00  96.00   1.00   50.00    --   27.00  57.00-180.00   90
  7  \w    -57.00  43.00   1.00   50.00    --  -27.15  77.00   0.00  100
  8  \w     -3.00  97.00   1.00   50.00    --   27.00  77.00  60.00  100
  9  \w     21.00 103.00   1.00   50.00    --   27.00-160.00 120.00   82
 10  \w      6.00  96.00   1.00   50.00    --   27.00  57.00-120.00   90
 11  \w    -97.00 -87.00   1.00   50.00    --  -27.15 -77.00 120.00   10
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0765021000
_diffrn_orient_matrix_UB_12      -0.0210608000
_diffrn_orient_matrix_UB_13      0.0374946000
_diffrn_orient_matrix_UB_21      -0.1682371000
_diffrn_orient_matrix_UB_22      0.0211629000
_diffrn_orient_matrix_UB_23      -0.0128740000
_diffrn_orient_matrix_UB_31      -0.0383877000
_diffrn_orient_matrix_UB_32      -0.0506593000
_diffrn_orient_matrix_UB_33      -0.0210007000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15431
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.503
_diffrn_reflns_theta_min         2.124
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       needle
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.649
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0628P)^2^+0.1681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2156
_reflns_number_total             2392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c01020_si_001.cif
_cod_data_source_block           5nI
_cod_depositor_comments
'Adding full bibliography for 4517840--4517846.cif.'
_cod_database_code               4517845
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C8H6N2O2
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.931
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C7(H7), C4(H4), C6(H6), C3(H3), C2(H2)
;
_shelx_res_checksum              54863
_shelx_hkl_checksum              9076
_olex2_date_sample_data_collection 2017-11-08
_olex2_submission_original_sample_id 5-Nitroindole
_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 1.601
_oxdiff_exptl_absorpt_empirical_full_min 0.382