Crystal structure of a tris(2-aminoethyl)methane capped carbamoylmethylphosphine oxide compound
Wackerle, Brandon G.; Werner, Eric J.; Staples, Richard J.; Biros, Shannon M.; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 993–996; doi:10.1107/S2056989024008478

data_2023241
_publ_section_title
;
 Crystal structure of a tris(2-aminoethyl)methane capped
 carbamoylmethylphosphine oxide compound
;
_journal_coeditor_code           VU2007
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              993
_journal_page_last               996
_journal_paper_doi               10.1107/S2056989024008478
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C25 H52 N3 O12 P3'
_chemical_formula_moiety         'C25 H52 N3 O12 P3'
_chemical_formula_sum            'C25 H52 N3 O12 P3'
_chemical_formula_weight         679.60
_chemical_name_systematic
'Diethyl {[(5-[2-(diethoxyphosphoryl)acetamido]-3-{2-[2-(diethoxyphosphoryl)acetamido]ethyl}pentyl)carbamoyl]methyl}phosphonate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                100.4792(11)
_cell_angle_beta                 100.1240(10)
_cell_angle_gamma                111.1313(11)
_cell_formula_units_Z            2
_cell_length_a                   10.02487(11)
_cell_length_b                   11.92992(15)
_cell_length_c                   16.6237(2)
_cell_measurement_reflns_used    13811
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.8460
_cell_measurement_theta_min      4.1040
_cell_volume                     1759.25(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.69a (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.69a (Oxford Diffraction, 2006)
;
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CrysAlisPro 1.171.42.69a (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
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CrystalMaker (Palmer, 2007)
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Olex2 (Dolomanov <i>et al.</i>, 2009; Bourhis <i>et al.</i>,
2015)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i>  (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy-S, Dualflex, HyPix-6000HE'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27502
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.209
_diffrn_reflns_theta_min         2.802
_exptl_absorpt_coefficient_mu    2.056
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       irregular
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0443P)^2^+0.5632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                6481
_reflns_number_total             7504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vu2007.cif
_cod_data_source_block           I
_cod_database_code               2023241
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.930
_shelx_hkl_checksum              37982
_shelx_res_checksum              30977