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_7129979
_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         'C54 H34 Cr2 O8 P2 Rh2, 2(C4 H8 O)'
_chemical_formula_sum            'C62 H50 Cr2 O10 P2 Rh2'
_chemical_formula_weight         1326.78
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-04 deposited with the CCDC.	2022-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.066(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8929(5)
_cell_length_b                   21.8724(11)
_cell_length_c                   9.5156(5)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    99.94
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      2.44
_cell_volume                     2676.6(2)
_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      99.94
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32385
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.625
_diffrn_reflns_theta_min         2.339
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1360 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.8508.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.592
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7491
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+8.1491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5982
_reflns_number_total             7491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01817a2.cif
_cod_data_source_block           yel144
_cod_database_code               7129979
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained planarity
 C12, C17, C16, C15, C14, C13
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C13A)
Uanis(C14) = Uanis(C14A)
Uanis(C16) = Uanis(C16A)
Uanis(C17) = Uanis(C17A)
4. Rigid body (RIGU) restrains
 O5, C1A, H1AA, H1AB, C1B, H1BA, H1BB, C1C, H1CA, H1CB, C1D, H1DA, H1DB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(H17A)=1-FVAR(1)
 Sof(H15)=Sof(C14)=Sof(H14)=Sof(C13)=Sof(H13)=Sof(C17)=Sof(H17)=Sof(C16)=
 Sof(H16)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13A(H13A), C14A(H14A), C15(H15A),
  C15(H15), C16A(H16A), C17A(H17A), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C14(H14), C13(H13), C17(H17), C16(H16)
6.d Fitted hexagon refined as free rotating group:
 C12(C13A,C14A,C15,C16A,C17A)
;
_shelx_res_checksum              88334
_olex2_submission_special_instructions 'No special instructions were received'