Conserved hydrogen bonding in tetrahydrocarbazolone derivatives: influence of solution-state assembly on crystal form nucleation
Robert M. Edkins; Elliott Hayden; Jonathan W. Steed; Katharina Fucke; Chem.Commun. 51 (2015) 5314–; doi:10.1039/C4cc10453F

data_7116792
_publ_section_title
;
 Conserved hydrogen bonding in tetrahydrocarbazolone derivatives:
 influence of solution-state assembly on crystal form nucleation
;
_journal_name_full               Chem.Commun.
_journal_page_first              5314
_journal_paper_doi               10.1039/C4cc10453F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C13 H13 N O'
_chemical_formula_sum            'C13 H13 N O'
_chemical_formula_weight         199.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_primary     iterative
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Olex2 1.2-alpha
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2014-12-23 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
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_cell_angle_alpha                90
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_cell_measurement_temperature    120
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
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_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9178
_diffrn_measurement_details
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  1 omega  -75.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366    0.0000   60.0000 116

  2 omega   33.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -137.0000 -134.0000 37

  3 omega  -43.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   38.0000  120.0000 67

  4 omega  -88.00   12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -77.0000    0.0000 100
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_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
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_diffrn_orient_matrix_UB_21      -0.0029402000
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_diffrn_orient_matrix_UB_23      0.0329714000
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
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_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.998
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear colourless'
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_exptl_crystal_density_diffrn    1.2980
_exptl_crystal_description       prism
_exptl_crystal_F_000             848.3694
_exptl_crystal_size_max          0.2674
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_refine_ls_d_res_high            0.7345
_refine_ls_d_res_low             7.3411
_refine_ls_goodness_of_fit_ref   1.3261
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.3261
_refine_ls_R_factor_all          0.2986
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_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_number_gt                1116
_reflns_number_total             2458
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4cc10453f2.cif
_cod_data_source_block           PCB_DMSO
_cod_original_cell_volume        2039.1(5)
_cod_database_code               7116792
_chemical_oxdiff_formula         'C13 H13 N O'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
The crystal is highly twinned but could not grown in any other way. Thus the residual electron
density is high and the Rint and final R-values are high as well.
;
_olex2_date_sample_data_collection 1336725831.94
_olex2_submission_special_instructions 'No special instructions were received'