Conformations of benzene-based tripodal isatin-bearing compounds in the crystalline state
Mazik, Monika; Schulze, Mathias M.; Schwarzer, Anke; CrystEngComm  (2017) –; doi:10.1039/C7CE00576H

data_7228377
_publ_section_title
;
 Conformations of benzene-based tripodal isatin-bearing compounds in the
 crystalline state
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00576H
_journal_year                    2017
_chemical_formula_moiety         'C39 H33 N3 O6, 1.5(C4 H10 O2)'
_chemical_formula_sum            'C45 H48 N3 O9'
_chemical_formula_weight         774.86
_chemical_name_common
;
 1,1',1''-(2,4,6-triethylbenzene-1,3,5-triyl)tris(methylene)
triindoline-2,3-dione
;
_chemical_name_systematic
;
 1,1',1''-(2,4,6-triethylbenzene-1,3,5-triyl)tris(methylene)
 triindoline-2,3-dione
;
_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   geom
_audit_creation_method           SHELXL-2012
_audit_update_record
;
2016-09-02 deposited with the CCDC.
2017-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.530(3)
_cell_angle_beta                 101.315(3)
_cell_angle_gamma                96.462(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7193(3)
_cell_length_b                   13.5370(5)
_cell_length_c                   17.0293(7)
_cell_measurement_reflns_used    35803
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      1.22
_cell_volume                     1957.42(13)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 2012), <i>publCIF</i> (Westrip, 2010), <i>SHELXLE</i>
 (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      ' 316 frames, detector distance = 120 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.220
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       plate
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0174(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         7674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0617P)^2^+1.3362P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6153
_reflns_number_total             7674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00576h2.cif
_cod_data_source_block           InKomp_06_masc039
_cod_database_code               7228377
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2012-9
_shelx_res_checksum              48025