Coordination isomerism in dioxophosphorane cyanides
Nasrullah, Ayu Afiqah; Zander, Edgar; Dankert, Fabian; Petrov, Andrey; Surkau, Jonas; Baráth, Eszter; Hering-Junghans, Christian; Chemical Science 16 (2025) 6909–6917; doi:10.1039/D4SC07636B

data_1574155
_publ_section_title
;
 Coordination isomerism in dioxophosphorane cyanides
;
_journal_issue                   16
_journal_name_full               'Chemical Science'
_journal_page_first              6909
_journal_page_last               6917
_journal_paper_doi               10.1039/D4SC07636B
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C41 H57 N Na O5, 0.5 (C7 H8)'
_chemical_formula_sum            'C44.5 H61 N Na O5 P'
_chemical_formula_weight         743.90
_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   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-11-07 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                70.73(3)
_cell_angle_beta                 77.25(3)
_cell_angle_gamma                75.49(3)
_cell_formula_units_Z            4
_cell_length_a                   14.468(3)
_cell_length_b                   17.705(4)
_cell_length_c                   18.868(4)
_cell_measurement_reflns_used    42801
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      1.73
_cell_volume                     4366.2(19)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2012)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'ORTEP-3v2020.1 (Farrugia, 2020)'
_computing_publication_material  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50613
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.323
_diffrn_reflns_theta_min         1.728
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'LANA (Stoe & Cie, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         23409
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0924P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13837
_reflns_number_total             23409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07636b3.cif
_cod_data_source_block           KS1613_DippTerPCN_Na_15_c_5_cmpd4
_cod_depositor_comments
'Adding full bibliography for 1574150--1574157.cif.'
_cod_original_cell_volume        4366.4(19)
_cod_original_formula_sum        'C44.50 H61 N Na O5 P'
_cod_database_code               1574155
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              64358