Two Modifications of Nitrilotris(methylenephenylphosphinic) Acid: A Polymeric Network with Intermolecular (O=P–O–H)3 vs. Monomeric Molecules with Intramolecular (O=P–O–H)3 Hydrogen Bond Cyclotrimers
Knerr, Steven; Brendler, Erica; Gericke, Robert; Kroke, Edwin; Wagler, Jörg; Crystals 14 (2024) 662–; doi:10.3390/cryst14070662

data_1572295
_publ_section_title
;
 Two Modifications of Nitrilotris(methylenephenylphosphinic) Acid: A
 Polymeric Network with Intermolecular (O=P--O--H)3 vs. Monomeric
 Molecules with Intramolecular (O=P--O--H)3 Hydrogen Bond Cyclotrimers
;
_journal_issue                   7
_journal_name_full               Crystals
_journal_page_first              662
_journal_paper_doi               10.3390/cryst14070662
_journal_volume                  14
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H24 N O6 P3'
_chemical_formula_sum            'C21 H24 N O6 P3'
_chemical_formula_weight         479.32
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ShelXT
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.2554(5)
_cell_length_b                   18.2554(5)
_cell_length_c                   11.4177(3)
_cell_measurement_reflns_used    16535
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.23
_cell_volume                     3295.28(15)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18163
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.993
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 773 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1748
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0398P)^2^+0.8406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                1669
_reflns_number_total             1748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            all-in-one-CIF.cif
_cod_data_source_block           sk-46_01
_cod_original_cell_volume        3295.3(2)
_cod_database_code               1572295
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              66000
_shelx_hkl_checksum              96002