Insight into the role of pre-assembly and desolvation in crystal nucleation: a case of <i>p</i>-nitrobenzoic acid
Zong, Shuyi; Wang, Jingkang; Wu, Hao; Liu, Qi; Hao, Yunhui; Huang, Xin; Wu, Dehui; Zhou, Guanchen; Hao, Hongxun; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619009478

data_2108488
_publ_section_title
;
 Insight into the role of pre-assembly and desolvation in crystal
 nucleation: a case of <i>p</i>-nitrobenzoic acid
;
_journal_coeditor_code           BM5112SUP1
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619009478
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         'C7 H5 N O4, C5 H9 N O'
_chemical_formula_sum            'C12 H14 N2 O5'
_chemical_formula_weight         266.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                98.844(4)
_cell_angle_beta                 102.693(4)
_cell_angle_gamma                100.077(5)
_cell_formula_units_Z            2
_cell_length_a                   7.1402(4)
_cell_length_b                   7.5689(4)
_cell_length_c                   11.9955(5)
_cell_measurement_reflns_used    5818
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      75.4590
_cell_measurement_theta_min      3.8370
_cell_volume                     610.09(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.957
_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   -119.00 -51.00   0.50    0.05    --  -46.62-167.00-156.00  136
  2  \w    -90.00 -14.00   0.50    0.05    --  -46.62 115.00  78.00  152
  3  \w   -123.00 -39.00   0.50    0.05    --  -46.62 167.00-136.00  168
  4  \w      8.00  90.00   0.50    0.05    --   46.62-115.00 -11.00  164
  5  \w     45.00 120.00   0.50    0.05    --   46.62 167.00-136.00  150
  6  \w   -158.00 -51.00   0.50    0.05    -- -100.00-167.00-156.00  214
  7  \w   -173.00 -85.00   0.50    0.05    -- -100.00-115.00 -11.00  176
  8  \w     35.00 146.00   0.50    0.05    --  107.75-167.00-156.00  222
  9  \w     35.00 113.00   0.50    0.05    --  107.75-115.00 -11.00  156
 10  \w     79.00 178.00   0.50    0.05    --  107.75 115.00  78.00  198
 11  \w   -120.00 -32.00   0.50    0.05    --  -46.62 -37.00 -60.00  176
 12  \w    -29.00  62.00   0.50    0.05    --   46.62 -19.00-180.00  182
 13  \w     23.00 120.00   0.50    0.05    --   46.62  77.00 150.00  194
 14  \w     33.00 123.00   0.50    0.05    --   46.62-167.00-156.00  180
 15  \w   -172.00 -85.00   0.50    0.05    -- -100.00 -45.00  60.00  174
 16  \w   -117.00 -27.00   0.50    0.05    -- -100.00  61.00 -60.00  180
 17  \w   -112.00 -27.00   0.50    0.05    -- -100.00 115.00  78.00  170
 18  \w   -175.00 -84.00   0.50    0.05    -- -100.00 -30.00 -60.00  182
 19  \w     93.00 178.00   0.50    0.05    --  107.75  45.00-180.00  170
 20  \w     35.00 122.00   0.50    0.05    --  107.75 -45.00 -60.00  174
 21  \w     35.00 109.00   0.50    0.05    --  107.75 -94.00-150.00  148
 22  \w     92.00 178.00   0.50    0.05    --  107.75  30.00  60.00  172
 23  \w     93.00 178.00   0.50    0.05    --  107.75  45.00 150.00  170
 24  \w     35.00 122.00   0.50    0.05    --  107.75 -45.00 120.00  174
 25  \w     35.00 122.00   0.50    0.05    --  107.75 -45.00-180.00  174
 26  \w     35.00 109.00   0.50    0.05    --  107.75 -94.00  60.00  148
 27  \w   -119.00 -68.00   0.50    0.05    --  -46.62 -57.00  90.00  102
 28  \w   -120.00 -32.00   0.50    0.05    --  -46.62 -37.00 120.00  176
 29  \w   -119.00 -23.00   0.50    0.05    --  -46.62 -77.00  60.00  192
 30  \w     23.00 120.00   0.50    0.05    --   46.62  77.00-150.00  194
 31  \w     23.00 120.00   0.50    0.05    --   46.62  77.00 -30.00  194
 32  \w     31.00 120.00   0.50    0.05    --   46.62  57.00 -90.00  178
;
_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      -0.1145547000
_diffrn_orient_matrix_UB_12      -0.1424579000
_diffrn_orient_matrix_UB_13      -0.1108937000
_diffrn_orient_matrix_UB_21      0.1151038000
_diffrn_orient_matrix_UB_22      0.1053561000
_diffrn_orient_matrix_UB_23      -0.0727708000
_diffrn_orient_matrix_UB_31      0.1579498000
_diffrn_orient_matrix_UB_32      -0.1145614000
_diffrn_orient_matrix_UB_33      0.0214579000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11217
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.516
_diffrn_reflns_theta_min         3.855
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
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    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0624P)^2^+0.2009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2064
_reflns_number_total             2448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bm5112sup1.cif
_cod_data_source_block           I.NMP
_cod_database_code               2108488
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.893
_reflns_odcompleteness_completeness 99.91
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C2(H2)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              97050
_shelx_hkl_checksum              44935
_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 2.966
_oxdiff_exptl_absorpt_empirical_full_min 0.536
_cod_database_fobs_code 2108488