Exceptionally large "through-space" nuclear spin coupling in a 2,4,6-tri(phosphanyl)-1,3,5-triphosphabenzene.
Meier, David C.; García-Romero, Álvaro; González-Pinardo, Daniel; Rees, Nicholas H.; Lovstedt, Alex; Fernández, Israel; Goicoechea, Jose M.; Chemical science 17 (2026) 544–554; doi:10.1039/d5sc07729j

data_1576156
_publ_section_title
;
 Exceptionally large "through-space" nuclear spin coupling in a
 2,4,6-tri(phosphanyl)-1,3,5-triphosphabenzene.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              544
_journal_page_last               554
_journal_paper_doi               10.1039/d5sc07729j
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C81 H114 N6 P6, C6 H14'
_chemical_formula_sum            'C87 H128 N6 P6'
_chemical_formula_weight         1443.77
_chemical_name_systematic
;
 [PCP{N(Dipp)CH2}2]3*hex
;
_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-2019/3
_audit_update_record
;
2025-07-31 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.626(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8201(5)
_cell_length_b                   21.8399(8)
_cell_length_c                   30.2910(10)
_cell_measurement_reflns_used    280
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      11.82
_cell_measurement_theta_min      2.46
_cell_volume                     8472.3(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS, 2019)'
_computing_data_collection       'BIS v6.2.14 (Bruker_AXS, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS, 2019)'
_computing_molecular_graphics
;
C. B. H\"ubschle, G. M. Sheldrick, B. Dittrich:
ShelXle: a Qt graphical user interface for SHELXL.
J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_publication_material  'APEX6 v2024.9-0 (Bruker AXS, 2024)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'Photon III'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2437
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            241826
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.409
_diffrn_reflns_theta_min         2.495
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_T_max  0.753055
_exptl_absorpt_correction_T_min  0.386067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
L. Krause, R. Herbst-Irmer, G.M. Sheldrick, D. Stalke:
Comparison of silver and molybdenum microfocus X-ray sources for 
single-crystal structure determination.
J. Appl. Cryst. (2015), 48, 3-10. doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         241826
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0763
_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^)+(0.1198P)^2^+4.2750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12878
_reflns_number_total             15559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07729j2.cif
_cod_data_source_block           24299
_cod_depositor_comments
'Adding full bibliography for 1576154--1576156.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1576156
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.684
_shelx_estimated_absorpt_t_max   0.804
_shelx_res_checksum              39228