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_7706463
_publ_section_title
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 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         'C38 H43 O11 P2 W2, C4 H12 N, C5 H12'
_chemical_formula_sum            'C47 H67 N O11 P2 W2'
_chemical_formula_weight         1251.65
_chemical_name_systematic        AS-457
_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
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-12-23
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2020-12-23 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                78.880(4)
_cell_angle_beta                 82.328(4)
_cell_angle_gamma                72.568(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9081(5)
_cell_length_b                   12.0080(5)
_cell_length_c                   21.9058(10)
_cell_measurement_reflns_used    38478
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.65
_cell_volume                     2677.3(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17719
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.823
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.406
_exptl_absorpt_correction_T_max  0.6399
_exptl_absorpt_correction_T_min  0.3896
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed 1.15'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       plank
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9493
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+3.7948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8701
_reflns_number_total             9493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04070c2.cif
_cod_data_source_block           6131
_cod_depositor_comments
'Adding full bibliography for 7706462--7706465.cif.'
_cod_database_code               7706463
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.504
_shelx_estimated_absorpt_t_min   0.300
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C45
 1.5 with sigma of 0.002
 C46-C47 = C45-C44 = C43-C44
 1.5 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C47 \\sim C46 \\sim C45 \\sim C44 \\sim C43: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C8) \\sim Ueq, Uanis(C8S) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9S)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C10S) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
4. Others
 Sof(C8S)=Sof(H8SA)=Sof(H8SB)=Sof(H8SC)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(H9SC)=
 Sof(C10S)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C6(H6), C16(H16), C18(H18), C20(H20)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8S(H8SA,H8SB,H8SC), C9(H9A,H9B,H9C), C9S(H9SA,H9SB,H9SC),
 C10(H10A,H10B,H10C), C10S(H10D,H10E,H10F), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 N(HA,HB,HC), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              76077
_olex2_submission_special_instructions 'No special instructions were received'