Synthesis and structure of 1,1',1''-[(2-bromo-eth-oxy)methane-tri-yl]tri-benzene and 1,1',1''-[(2-iodoeth-oxy)methane-tri-yl]tri-benzene.
Fischer, Julian; Hebenbrock, Marian; Acta crystallographica. Section E, Crystallographic communications 81 (2025) 214–218; doi:10.1107/S2056989025001124

data_2023402
_publ_section_title
;
 Synthesis and structure of
 1,1',1''-[(2-bromo-eth-oxy)methane-tri-yl]tri-benzene and
 1,1',1''-[(2-iodoeth-oxy)methane-tri-yl]tri-benzene.
;
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
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_journal_page_last               218
_journal_paper_doi               10.1107/S2056989025001124
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          'C21 H19 I O'
_chemical_formula_moiety         'C21 H19 I O'
_chemical_formula_sum            'C21 H19 I O'
_chemical_formula_weight         414.26
_chemical_name_systematic
;
1,1',1''-[(2-Iodoethoxy)methanetriyl]tribenzene
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
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_cell_angle_alpha                90
_cell_angle_beta                 105.9450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3500(6)
_cell_length_b                   10.5936(3)
_cell_length_c                   17.5475(6)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.21
_cell_volume                     3458.60(19)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2021)
;
_computing_data_collection
;
<i>APEX4</i> (Bruker, 2021)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2021)
;
_computing_molecular_graphics
;
SHELXTL (sheldrick, 2008)
;
_computing_publication_material
;
<i>APEX4</i> (Bruker, 2021), <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/1</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
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'Bruker D8 Venture with Photon III CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    1.854
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5064
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
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_refine_diff_density_min         -0.677
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         7929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+2.7021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0538
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yy2014.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2023401--2023402.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023402
_shelx_estimated_absorpt_t_min   0.408
_shelx_estimated_absorpt_t_max   0.708
_shelx_hkl_checksum              12652
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