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_7706462
_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         'C39 H47 N O10 P2 W2'
_chemical_formula_sum            'C39 H47 N O10 P2 W2'
_chemical_formula_weight         1119.41
_chemical_name_systematic        AS-358
_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                67.727(5)
_cell_angle_beta                 66.395(5)
_cell_angle_gamma                70.170(5)
_cell_formula_units_Z            1
_cell_length_a                   9.8761(18)
_cell_length_b                   10.9209(19)
_cell_length_c                   12.138(2)
_cell_measurement_reflns_used    5559
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.84
_cell_measurement_theta_min      2.31
_cell_volume                     1082.6(3)
_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 0.997
_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  0.1006
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30838
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.493
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.435
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4878
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1344 before and 0.0820 after correction. The Ratio of minimum to maximum transmission is 0.6538. 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    1.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.249
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0278P)^2^+4.9975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4401
_reflns_number_total             5213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04070c2.cif
_cod_data_source_block           5820f
_cod_depositor_comments
'Adding full bibliography for 7706462--7706465.cif.'
_cod_original_cell_volume        1082.7(3)
_cod_database_code               7706462
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.395
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H(0.5) N(0.5) HA(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N(HA), C2(H2), C4(H4), C6(H6)
4.b 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), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              81501
_olex2_submission_special_instructions 'No special instructions were received'