Synthesis, spectroscopic analysis and crystal structure of (<i>N</i>-{2-[(2-amino-eth-yl)amino]-eth-yl}-4'-methyl-[1,1'-biphenyl]-4-sulfonamidato)tri-carb-on-ylrhenium(I).
Kaluthanthiri, Dinithi; Perera, Theshini; Fronczek, Frank R.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 742–745; doi:10.1107/S2056989024005656

data_2023164
_publ_section_title
;
 Synthesis, spectroscopic analysis and crystal structure of
 (<i>N</i>-{2-[(2-amino-eth-yl)amino]-eth-yl}-4'-methyl-[1,1'-biphenyl]-4-sulfonamidato)tri-carb-on-ylrhenium(I).
;
_journal_coeditor_code           VM2303
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              742
_journal_page_last               745
_journal_paper_doi               10.1107/S2056989024005656
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Re (C17 H22 N3 O2 S) (C O)3]'
_chemical_formula_moiety         'C20 H22 N3 O5 Re S'
_chemical_formula_sum            'C20 H22 N3 O5 Re S'
_chemical_formula_weight         602.66
_chemical_name_systematic
(<i>N</i>-{2-[(2-Aminoethyl)amino]ethyl}-4'-methyl-[1,1'-biphenyl]-4-sulfonamidato)tricarbonylrhenium(I)
_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
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 95.472(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5651(9)
_cell_length_b                   7.6604(4)
_cell_length_c                   15.4897(11)
_cell_measurement_reflns_used    2346
_cell_measurement_temperature    296
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      2.6
_cell_volume                     2192.8(2)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            119413
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.176
_diffrn_reflns_theta_min         1.102
_exptl_absorpt_coefficient_mu    5.672
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_description       needle
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.002
_refine_diff_density_min         -1.800
_refine_ls_extinction_coef       0.00017(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2017/1</i> (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0179P)^2^+6.5423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                3513
_reflns_number_total             4849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2303.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023164.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023164
_shelx_estimated_absorpt_t_min   0.368
_shelx_estimated_absorpt_t_max   0.765
_shelx_hkl_checksum              68732
_shelx_res_checksum              15090