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_1572296
_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_formula_moiety         'C30 H48 N O6 P3 Si3'
_chemical_formula_sum            'C30 H48 N O6 P3 Si3'
_chemical_formula_weight         695.87
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_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            12
_cell_length_a                   12.1818(3)
_cell_length_b                   12.1818(3)
_cell_length_c                   92.431(3)
_cell_measurement_reflns_used    19394
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.22
_cell_volume                     11878.8(6)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       109
_diffrn_reflns_limit_l_min       -109
_diffrn_reflns_number            25515
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.223
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.6603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3464
_reflns_number_total             4686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            all-in-one-CIF.cif
_cod_data_source_block           sk-54-2s_05
_cod_original_cell_volume        11878.8(7)
_cod_database_code               1572296
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.960
_shelx_res_checksum              16982
_shelx_hkl_checksum              78926