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_1574157
_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         'C43 H61 K N O8 P, 2(C7 H8)'
_chemical_formula_sum            'C57 H77 K N O8 P'
_chemical_formula_weight         974.26
_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_date             2024-10-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-11-07 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                98.680(2)
_cell_angle_beta                 90.422(2)
_cell_angle_gamma                110.288(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4129(4)
_cell_length_b                   14.6924(6)
_cell_length_c                   19.2865(8)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      2.32
_cell_measurement_theta_min      66.51
_cell_volume                     2730.22(19)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55387
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.630
_diffrn_reflns_theta_max         66.630
_diffrn_reflns_theta_min         2.322
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_T_max  0.8642
_exptl_absorpt_correction_T_min  0.7679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         9646
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0574P)^2^+0.3910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8242
_reflns_number_total             9646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07636b3.cif
_cod_data_source_block
ax2705abs_a-cn_DippTerPO2_CN_NC_K_18-c-6_cmpd2O2
_cod_depositor_comments
'Adding full bibliography for 1574150--1574157.cif.'
_cod_database_code               1574157
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.699
_olex2_refinement_description
;
1. Shared sites
{C31, N1A}
{N1, C31A}
2. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(N1A)
Uanis(N1) = Uanis(C31A)
Uanis(C50A) = Uanis(C50B)
3. Same fragment restrains
{C44A, C45A, C46A, C47A, C48A, C49A, C50A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C44B, C45B, C46B, C47B, C48B, C49B, C50B}
4. Others
 Sof(C44B)=Sof(C45B)=Sof(H45B)=Sof(C46B)=Sof(H46B)=Sof(C47B)=Sof(H47B)=
 Sof(C48B)=Sof(H48B)=Sof(C49B)=Sof(H49B)=Sof(C50B)=Sof(H50D)=Sof(H50E)=
 Sof(H50F)=1-FVAR(1)
 Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=
 Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(H50B)=
 Sof(H50C)=FVAR(1)
 Sof(N1A)=Sof(C31A)=1-FVAR(2)
 Sof(C31)=Sof(N1)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22),
 C23(H23), C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A), C49A(H49A),
 C45B(H45B), C46B(H46B), C47B(H47B), C48B(H48B), C49B(H49B), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C50A(H50A,H50B,H50C), C50B(H50D,H50E,H50F), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              64632
_olex2_submission_special_instructions 'No special instructions were received'