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_1574153
_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 O7 P, 2(C7 H8)'
_chemical_formula_sum            'C55 H73 N Na O7 P'
_chemical_formula_weight         914.10
_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                92.40(3)
_cell_angle_beta                 107.37(3)
_cell_angle_gamma                91.81(3)
_cell_formula_units_Z            2
_cell_length_a                   12.760(3)
_cell_length_b                   12.763(3)
_cell_length_c                   16.898(3)
_cell_measurement_reflns_used    44016
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      1.60
_cell_measurement_theta_min      29.60
_cell_volume                     2621.3(11)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2012)'
_computing_data_reduction        X-AREA
_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)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43845
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.388
_diffrn_reflns_theta_min         1.599
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'LANA (Stoe & Cie, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         14197
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0768P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9792
_reflns_number_total             14197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07636b3.cif
_cod_data_source_block           ks1605-cn_DippTerPO2_CN_NC_Na_15-c-5_cmpd4O2
_cod_depositor_comments
'Adding full bibliography for 1574150--1574157.cif.'
_cod_original_cell_volume        2621.4(10)
_cod_database_code               1574153
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1. Shared sites
{N1, C31A}
{N1A, C31}
2. Others
 Fixed Uiso: H3(0.041) H4(0.043) H5(0.039) H9(0.051) H10(0.055) H11(0.051)
 H13(0.05) H14A(0.101) H14B(0.101) H14C(0.101) H15A(0.095) H15B(0.095)
 H15C(0.095) H16(0.047) H17A(0.072) H17B(0.072) H17C(0.072) H18A(0.072)
 H18B(0.072) H18C(0.072) H21(0.048) H22(0.053) H23(0.052) H25(0.049) H26A(0.08)
 H26B(0.08) H26C(0.08) H27A(0.134) H27B(0.134) H27C(0.134) H28(0.054)
 H29A(0.094) H29B(0.094) H29C(0.094) H30A(0.084) H30B(0.084) H30C(0.084)
 H32A(0.078) H32B(0.078) H33A(0.079) H33B(0.079) H34A(0.094) H34B(0.094)
 H35A(0.096) H35B(0.096) H36A(0.084) H36B(0.084) H37A(0.068) H37B(0.068)
 H38A(0.054) H38B(0.054) H39A(0.052) H39B(0.052) H40A(0.077) H40B(0.077)
 H41A(0.083) H41B(0.083) H32C(0.078) H32D(0.078) H33C(0.084) H33D(0.084)
 H34C(0.065) H34D(0.065) H35C(0.061) H35D(0.061) H36C(0.061) H36D(0.061)
 H37C(0.061) H37D(0.061) H38C(0.078) H38D(0.078) H39C(0.079) H39D(0.079)
 H40C(0.094) H40D(0.094) H41C(0.096) H41D(0.096) H51(0.07) H52(0.07) H53(0.07)
 H54(0.067) H55(0.066) H56A(0.133) H56B(0.133) H56C(0.133) H61A(0.075)
 H62A(0.08) H63A(0.076) H64A(0.067) H65A(0.068) H66A(0.129) H66B(0.129)
 H66C(0.129) H61B(0.063) H62B(0.08) H63B(0.082) H64B(0.069) H65B(0.053)
 H66D(0.131) H66E(0.131) H66F(0.131)
 Fixed X: H3(0.640948) H4(0.522165) H5(0.456041) H9(0.983624) H10(0.928305)
 H11(0.742735) H13(0.802365) H14A(1.001893) H14B(0.955216) H14C(0.890358)
 H15A(0.889208) H15B(0.956578) H15C(1.000505) H16(0.52127) H17A(0.541217)
 H17B(0.447138) H17C(0.566328) H18A(0.571694) H18B(0.455068) H18C(0.55929)
 H21(0.580014) H22(0.393493) H23(0.266811) H25(0.703841) H26A(0.751833)
 H26B(0.833603) H26C(0.72795) H27A(0.68992) H27B(0.807188) H27C(0.71052)
 H28(0.327606) H29A(0.166694) H29B(0.166903) H29C(0.257439) H30A(0.178318)
 H30B(0.273337) H30C(0.175091) H32A(0.599873) H32B(0.642568) H33A(0.611835)
 H33B(0.498818) H34A(0.447943) H34B(0.461685) H35A(0.625464) H35B(0.541146)
 H36A(0.688213) H36B(0.762584) H37A(0.863737) H37B(0.775488) H38A(0.881909)
 H38B(0.9872) H39A(1.017913) H39B(1.027813) H40A(0.953875) H40B(0.948327)
 H41A(0.815421) H41B(0.763044) H32C(0.874668) H32D(0.968684) H33C(1.017261)
 H33D(1.02877) H34C(0.9859) H34D(0.97589) H35C(0.8601) H35D(0.79719)
 H36C(0.635666) H36D(0.689678) H37C(0.640705) H37D(0.535671) H38C(0.445463)
 H38D(0.464003) H39C(0.626727) H39D(0.527864) H40C(0.660801) H40D(0.742809)
 H41C(0.829441) H41D(0.740475) H51(0.105073) H52(0.260964) H53(0.246461)
 H54(0.073048) H55(-0.082403) H56A(-0.085713) H56B(-0.154911) H56C(-0.146264)
 H61A(0.282691) H62A(0.302824) H63A(0.246096) H64A(0.169492) H65A(0.146446)
 H66A(0.222867) H66B(0.116489) H66C(0.235054) H61B(0.183105) H62B(0.142548)
 H63B(0.169944) H64B(0.240308) H65B(0.272379) H66D(0.285654) H66E(0.314484)
 H66F(0.19127)
 Fixed Y: H3(0.822527) H4(0.699527) H5(0.553274) H9(0.884604) H10(1.046726)
 H11(1.078728) H13(0.666678) H14A(0.767308) H14B(0.653637) H14C(0.755754)
 H15A(0.646894) H15B(0.589639) H15C(0.701248) H16(0.887879) H17A(0.999167)
 H17B(1.039673) H17C(1.098033) H18A(1.067582) H18B(1.004591) H18C(0.949961)
 H21(0.254109) H22(0.209556) H23(0.338996) H25(0.509004) H26A(0.305732)
 H26B(0.407636) H26C(0.402007) H27A(0.430274) H27B(0.406895) H27C(0.317517)
 H28(0.610997) H29A(0.452994) H29B(0.574935) H29C(0.50224) H30A(0.486036)
 H30B(0.562527) H30C(0.610154) H32A(0.503396) H32B(0.467211) H33A(0.647226)
 H33B(0.584936) H34A(0.801992) H34B(0.763334) H35A(0.855063) H35B(0.934065)
 H36A(1.030716) H36B(0.967001) H37A(1.015267) H37B(0.949321) H38A(0.822506)
 H38B(0.88467) H39A(0.734646) H39B(0.707723) H40A(0.513444) H40B(0.58055)
 H41A(0.442936) H41B(0.486133) H32C(0.850126) H32D(0.91682) H33C(0.764238)
 H33D(0.748272) H34C(0.544178) H34D(0.592784) H35C(0.439356) H35D(0.490882)
 H36C(0.474758) H36D(0.435569) H37C(0.600962) H37D(0.526006) H38C(0.745593)
 H38D(0.697492) H39C(0.802364) H39D(0.876619) H40C(1.011635) H40D(0.94128)
 H41C(1.015401) H41D(0.952319) H51(0.77697) H52(0.782525) H53(0.770312)
 H54(0.74983) H55(0.742467) H56A(0.759513) H56B(0.809007) H56C(0.684433)
 H61A(0.81569) H62A(0.765335) H63A(0.872606) H64A(1.03023) H65A(1.081114)
 H66A(0.930368) H66B(0.991928) H66C(1.051522) H61B(1.018925) H62B(1.130425)
 H63B(1.083143) H64B(0.925321) H65B(0.804669) H66D(0.761973) H66E(0.860803)
 H66F(0.811712)
 Fixed Z: H3(1.011474) H4(1.042079) H5(0.951967) H9(0.938943) H10(0.888411)
 H11(0.837381) H13(0.948606) H14A(1.052566) H14B(1.065754) H14C(1.077023)
 H15A(0.845551) H15B(0.926391) H15C(0.906368) H16(0.818853) H17A(0.937104)
 H17B(0.860199) H17C(0.889324) H18A(0.739222) H18B(0.714655) H18C(0.699787)
 H21(0.796431) H22(0.745512) H23(0.734585) H25(0.863424) H26A(0.810689)
 H26B(0.831502) H26C(0.751087) H27A(0.981977) H27B(0.970553) H27C(0.945752)
 H28(0.797178) H29A(0.802853) H29B(0.829168) H29C(0.884323) H30A(0.664629)
 H30B(0.652238) H30C(0.680882) H32A(0.525875) H32B(0.448946) H33A(0.399189)
 H33B(0.395935) H34A(0.482503) H34B(0.395062) H35A(0.421927) H35B(0.443697)
 H36A(0.561217) H36B(0.516419) H37A(0.65578) H37B(0.687315) H38A(0.750982)
 H38B(0.739328) H39A(0.660116) H39B(0.754111) H40A(0.667338) H40B(0.588127)
 H41A(0.552078) H41B(0.621789) H32C(0.747729) H32D(0.723212) H33C(0.66319)
 H33D(0.759065) H34C(0.700769) H34D(0.612756) H35C(0.593096) H35D(0.653459)
 H36C(0.545304) H36D(0.47527) H37C(0.409987) H37D(0.406974) H38C(0.473255)
 H38D(0.389675) H39C(0.414087) H39D(0.415376) H40C(0.523868) H40D(0.49055)
 H41C(0.626842) H41D(0.658754) H51(0.530664) H52(0.48826) H53(0.347413)
 H54(0.249159) H55(0.292164) H56A(0.504158) H56B(0.420016) H56C(0.42424)
 H61A(0.75439) H62A(0.887362) H63A(0.979872) H64A(0.938411) H65A(0.80534)
 H66A(0.647524) H66B(0.650085) H66C(0.678738) H61B(0.917956) H62B(0.813446)
 H63B(0.686746) H64B(0.669287) H65B(0.770516) H66D(0.910062) H66E(0.975522)
 H66F(0.942296)
;
_shelx_res_checksum              66964
_olex2_submission_special_instructions 'No special instructions were received'