Molecular 1,1'-bifunctional mixed-valence P-P compounds, enabled through metal complexation.
Schmer, Alexander; Bauza, Antonio; Schnakenburg, Gregor; Frontera, Antonio; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2131–2137; doi:10.1039/d0dt04070c

data_7706464
_publ_section_title
;
 Molecular 1,1'-bifunctional mixed-valence P-P compounds, enabled through
 metal complexation.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2131
_journal_page_last               2137
_journal_paper_doi               10.1039/d0dt04070c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C46 H59 Li O15 P2 W2, C4 H10 O'
_chemical_formula_sum            'C50 H69 Li O16 P2 W2'
_chemical_formula_weight         1362.63
_chemical_name_systematic        AS-418-2
_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   mixed
_audit_creation_date             2020-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2020-08-05 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                100.106(3)
_cell_angle_beta                 98.870(4)
_cell_angle_gamma                99.627(3)
_cell_formula_units_Z            4
_cell_length_a                   12.8111(6)
_cell_length_b                   20.0384(6)
_cell_length_c                   22.5678(7)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.32
_cell_measurement_theta_min      2.45
_cell_volume                     5521.8(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1852
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            126588
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.545
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.286
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3853
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1556 before and 0.0866 after correction. The Ratio of minimum to maximum transmission is 0.5165. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       plate
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         7.020
_refine_diff_density_min         -5.374
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1310
_refine_ls_number_reflns         19977
_refine_ls_number_restraints     590
_refine_ls_restrained_S_all      1.281
_refine_ls_R_factor_all          0.1587
_refine_ls_R_factor_gt           0.1337
_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^)+(0.0001P)^2^+417.4732P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2269
_refine_ls_wR_factor_ref         0.2383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15782
_reflns_number_total             19977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04070c2.cif
_cod_data_source_block           6174
_cod_depositor_comments
'Adding full bibliography for 7706462--7706465.cif.'
_cod_database_code               7706464
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22'-C21' = C20'-C19' = C18'-C17' = C16'-C15' = C18-C17
 1.5 with sigma of 0.001
 O2'-C15' = O3'-C16' = O3'-C17' = O4'-C18' = O4'-C19' = O5'-C20'
 1.39 with sigma of 0.01
 C21'-C20'
 2.3 with sigma of 0.01
 O2'-C22'
 1.4 with sigma of 0.01
 C48-C47 = C50-C49 = C48'-C47' = C50'-C49'
 1.5 with sigma of 0.01
 O16'-C48' = O16'-C49' = O16-C48
 1.39 with sigma of 0.01
 P2'-Li'
 3.16 with sigma of 0.01
 P2-H2
 1.43 with sigma of 0.01
 P2'-H2'
 1.43 with sigma of 0.01
3. Rigid bond restraints
 C11', C13'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7', C8'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11', C14'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C22' \\sim O2' \\sim C15' \\sim C16' \\sim C17' \\sim C18' \\sim C19' \\sim
C20' \\sim C21' \\sim O5' \\sim O4' \\sim O3': within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004
O10 \\sim C41 \\sim C38 \\sim O7 \\sim C39 \\sim O8 \\sim C40 \\sim O9 \\sim
C37 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
O7' \\sim C38' \\sim C41' \\sim O10' \\sim C37' \\sim O6' \\sim O9' \\sim C40'
\\sim C39' \\sim O8': within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(C16') \\sim Ueq, Uanis(C15') \\sim Ueq, Uanis(C43') \\sim Ueq,
Uanis(C42') \\sim Ueq, Uanis(C46') \\sim Ueq, Uanis(C45') \\sim Ueq,
Uanis(C39') \\sim Ueq, Uanis(C40') \\sim Ueq, Uanis(C37') \\sim Ueq,
Uanis(C22') \\sim Ueq, Uanis(C44') \\sim Ueq, Uanis(C21') \\sim Ueq,
Uanis(O13') \\sim Ueq, Uanis(C23') \\sim Ueq, Uanis(C28') \\sim Ueq,
Uanis(C29') \\sim Ueq, Uanis(C1') \\sim Ueq, Uanis(C19') \\sim Ueq, Uanis(C17')
\\sim Ueq, Uanis(C5') \\sim Ueq, Uanis(C13') \\sim Ueq, Uanis(O16') \\sim Ueq,
Uanis(C27') \\sim Ueq, Uanis(C14') \\sim Ueq, Uanis(C34') \\sim Ueq,
Uanis(C33') \\sim Ueq, Uanis(C31') \\sim Ueq, Uanis(C32') \\sim Ueq,
Uanis(C30') \\sim Ueq, Uanis(C24') \\sim Ueq, Uanis(C26') \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C6') \\sim Ueq, Uanis(C4') \\sim Ueq, Uanis(C12')
\\sim Ueq, Uanis(C9') \\sim Ueq, Uanis(C7') \\sim Ueq, Uanis(C11') \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C50') \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C18')
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O6') \\sim Ueq, Uanis(O7') \\sim Ueq, Uanis(C16') \\sim Ueq, Uanis(C15')
\\sim Ueq, Uanis(C18') \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(O14') \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C41) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C38') \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O16) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Li') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O11') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Ternary CH refined with riding coordinates:
 P2'(H2')
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C15'(H15C,H15D),
 C16'(H16C,H16D), C17'(H17C,H17D), C18'(H18C,H18D), C19'(H19C,H19D), C20'(H20C,
 H20D), C21'(H21C,H21D), C22'(H22C,H22D), C48(H48A,H48B), C49(H49A,H49B),
 C48'(H48C,H48D), C49'(H49C,H49D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C6(H6), C24(H24), C26(H26), C28(H28), C2'(H2'A), C4'(H4'),
 C6'(H6'), C24'(H24'), C26'(H26'), C28'(H28')
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C8'(H8'A,H8'B,H8'C), C9'(H9'A,H9'B,H9'C), C10'(H10D,H10E,H10F),
 C12'(H12D,H12E,H12F), C13'(H13D,H13E,H13F), C14'(H14D,H14E,H14F), C30'(H30D,
 H30E,H30F), C31'(H31D,H31E,H31F), C32'(H32D,H32E,H32F), C34'(H34D,H34E,H34F),
 C35'(H35D,H35E,H35F), C36'(H36D,H36E,H36F), C47(H47A,H47B,H47C), C50(H50A,H50B,
 H50C), C47'(H47D,H47E,H47F), C50'(H50D,H50E,H50F)
;
_shelx_res_checksum              5607
_olex2_submission_special_instructions 'No special instructions were received'