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_7228378
_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         'C42 H39 N3 O6, C2 H3 N'
_chemical_formula_sum            'C44 H42 N4 O6'
_chemical_formula_weight         722.81
_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      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                 112.7102(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9687(5)
_cell_length_b                   8.5086(2)
_cell_length_c                   24.4790(6)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.50
_cell_volume                     3644.53(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            47755
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.900
_diffrn_reflns_theta_min         2.951
_exptl_absorpt_coefficient_mu    0.088
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         8703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+3.6140P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7707
_reflns_number_total             8703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00576h2.cif
_cod_data_source_block           Schulze_19_0m
_cod_database_code               7228378
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2012-9
_shelx_res_checksum              580