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_7228379
_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, C2 H3 N'
_chemical_formula_sum            'C39.83 H34.25 N3.42 O6'
_chemical_formula_weight         656.66
_chemical_name_common
;
 1,1',1''-((2,4,6-trimethylbenzene-1,3,5-triyl)
tris(methylene))tris(5-methylindoline-2,3-dione)
;
_chemical_name_systematic
;
 1,1',1''-((2,4,6-trimethylbenzene-1,3,5-triyl)
tris(methylene))tris(5-methylindoline-2,3-dione)
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 102.591(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9390(7)
_cell_length_b                   11.9019(7)
_cell_length_c                   17.5127(9)
_cell_measurement_reflns_used    11231
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.08
_cell_volume                     3242.3(3)
_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      150(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      ' 222 frames, detector distance = 120 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_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  0.1589
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27972
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.085
_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    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       piece
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0062(7)
_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   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1505
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0280P)^2^+2.6941P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3396
_reflns_number_total             6362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00576h2.cif
_cod_data_source_block           Ing17_Am_ACN_masc046
_cod_database_code               7228379
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2012-9
_shelx_res_checksum              81912