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_7706465
_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_absolute_configuration ad
_chemical_formula_moiety         'C43 H55 N O10 P2 W2, C4 H9 O'
_chemical_formula_sum            'C47 H64 N O11 P2 W2'
_chemical_formula_weight         1248.63
_chemical_name_systematic        AS-401
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-02-27
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5701(14)
_cell_length_b                   22.718(3)
_cell_length_c                   24.433(3)
_cell_measurement_reflns_used    6077
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.03
_cell_measurement_theta_min      2.29
_cell_volume                     5312.1(12)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1622
_diffrn_reflns_av_unetI/netI     0.1086
_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       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            83420
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.657
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.441
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4928
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1389 before and 0.1055 after correction. The Ratio of minimum to maximum transmission is 0.6604. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       needle
_exptl_crystal_F_000             2476
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.584
_refine_diff_density_min         -2.851
_refine_diff_density_rms         0.224
_refine_ls_abs_structure_details
;
 Flack x determined using 3537 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         12809
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0383P)^2^+0.3764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9739
_reflns_number_total             12809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04070c2.cif
_cod_data_source_block           5908g
_cod_depositor_comments
'Adding full bibliography for 7706462--7706465.cif.'
_cod_database_code               7706465
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.298
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(C20) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C37) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C19) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
3.a Riding coordinates:
 N(H)
3.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C16(H16), C18(H18), C20(H20), C46(H46)
3.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), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              1733
_olex2_submission_special_instructions 'No special instructions were received'