Highly Flexible Phosphabenzenes: A Missing Coordination Mode of 2,4,6-Triaryl-λ3-Phosphinines
Yue, Erlin; Petrov, Andrey; Frost, Daniel Sebastian; Dettling, Lea; Conrad, Lawrence; Wossidlo, Friedrich; Coles, Nathan Thomas; Weber, Manuela; Muller, Christian; Chemical Communications  (2022) –; doi:10.1039/D2CC01817A

data_7129980
_publ_section_title
;
 Highly Flexible Phosphabenzenes: A Missing Coordination Mode of
 2,4,6-Triaryl-\l3-Phosphinines
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01817A
_journal_year                    2022
_chemical_formula_moiety         'C60 H46 Cr2 O8 P2 Rh2'
_chemical_formula_sum            'C60 H46 Cr2 O8 P2 Rh2'
_chemical_formula_weight         1266.73
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2021-10-04 deposited with the CCDC.	2022-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.404(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0219(5)
_cell_length_b                   9.5027(3)
_cell_length_c                   23.0919(9)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.60
_cell_volume                     3026.31(19)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28648
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.536
_diffrn_reflns_theta_min         2.323
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1118 before and 0.0441 after correction.
The Ratio of minimum to maximum transmission is 0.8770.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1276
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O, DCM'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         8170
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+3.4939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6794
_reflns_number_total             8170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01817a2.cif
_cod_data_source_block           ap019
_cod_database_code               7129980
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.730
_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. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C18A)
Uanis(C17) = Uanis(C17A)
Uanis(C14) = Uanis(C14A)
Uanis(C15) = Uanis(C15A)
3. Rigid body (RIGU) restrains
 C13, C18, C17, C16, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14A, C15A, C16, C17A, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17A)=Sof(C15A)=Sof(H15A)=Sof(C14A)=
 Sof(H14A)=1-FVAR(1)
 Sof(C18)=Sof(H18)=Sof(C17)=Sof(H17)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C18A(H18A), C17A(H17A), C15A(H15A),
 C14A(H14A), C18(H18), C17(H17), C15(H15), C14(H14), C21(H21), C22(H22),
 C24(H24), C25(H25)
5.c Fitted hexagon refined as free rotating group:
 C13(C18A,C17A,C16,C15A,C14A)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4054
_shelx_fab_checksum              52600
_olex2_submission_special_instructions 'No special instructions were received'