A carbene-stabilized diphosphorus: a triple-bonded diphosphorus (P[triple bond, length as m-dash]P) and a bis(phosphinidene) (P-P) transfer agent.
Yoon, Joseph S.; Abdellaoui, Mehdi; Gembicky, Milan; Bertrand, Guy; Chemical science 15 (2024) 15713–15716; doi:10.1039/d4sc05091f

data_1572481
_publ_section_title
;
 A carbene-stabilized diphosphorus: a triple-bonded diphosphorus (P[triple
 bond, length as m-dash]P) and a bis(phosphinidene) (P-P) transfer agent.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              15713
_journal_page_last               15716
_journal_paper_doi               10.1039/d4sc05091f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C14 H30 N2 P2'
_chemical_formula_sum            'C14 H30 N2 P2'
_chemical_formula_weight         288.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.731(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7119(16)
_cell_length_b                   11.7054(15)
_cell_length_c                   14.533(2)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.57
_cell_volume                     1823.9(4)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2019)'
_computing_data_collection       'APEX5 v2023.9-2 (Bruker, 2023)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon III Area Detector'
_diffrn_detector_area_resol_mean 7.407
_diffrn_detector_type            'CPAD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            79435
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.560
_diffrn_reflns_theta_min         2.576
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.5547
_exptl_absorpt_correction_T_min  0.5293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1348 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.9542.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       plank
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3363
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+1.1604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2679
_reflns_number_total             3363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05091f2.cif
_cod_data_source_block           bis(carbene)p2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1572478--1572481.cif.
;
_cod_original_cell_volume        1824.0(4)
_cod_database_code               1572481
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Same fragment restrains
{P1, P2, N1, N2, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14}
sigma for 1-2: 0.02, 1-3: 0.04
as in
{P1', P2', N1', N2', C1', C2', C3', C4', C5', C6', C7', C8', C9', C10', C11',
C12', C13', C14'}
4. Others
 Sof(P1')=Sof(P2')=Sof(N1')=Sof(N2')=Sof(C1')=Sof(H1')=Sof(C2')=Sof(H2')=
 Sof(C3')=Sof(H3'A)=Sof(H3'B)=Sof(H3'C)=Sof(C4')=Sof(H4')=Sof(C5')=Sof(H5'A)=
 Sof(H5'B)=Sof(H5'C)=Sof(C6')=Sof(H6'A)=Sof(H6'B)=Sof(H6'C)=Sof(C7')=Sof(H7')=
 Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=
 Sof(C10')=Sof(H10')=Sof(C11')=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12')=
 Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13')=Sof(H13')=Sof(C14')=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(P1)=Sof(P2)=Sof(N1)=Sof(N2)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=
 Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C13(H13), C4'(H4'), C7'(H7'), C10'(H10'), C13'(H13')
5.b Aromatic/amide H refined with riding coordinates:
 C1'(H1'), C2'(H2')
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C3'(H3'A,H3'B,H3'C), C5'(H5'A,H5'B,H5'C), C6'(H6'A,H6'B,H6'C), C8'(H8'A,H8'B,
 H8'C), C9'(H9'A,H9'B,H9'C), C11'(H11D,H11E,H11F), C12'(H12D,H12E,H12F),
 C14'(H14D,H14E,H14F)
;
_shelx_res_checksum              23146
_shelx_hkl_checksum              74382
_olex2_submission_special_instructions 'No special instructions were received'