Syntheses and structures of dimesitylphosphinite complexes of alkali metals and their catalytic activity in hydrophosphorylation reactions.
Fener, Benjamin E.; Schüler, Philipp; Liebing, Phil; Görls, Helmar; Westerhausen, Matthias; Dalton transactions (Cambridge, England : 2003) 54 (2024) 181–197; doi:10.1039/d4dt02721c

data_7717344
_publ_section_title
;
 Syntheses and structures of dimesitylphosphinite complexes of alkali
 metals and their catalytic activity in hydrophosphorylation reactions.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              181
_journal_page_last               197
_journal_paper_doi               10.1039/d4dt02721c
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C60 H92 O2 P2 Rb2'
_chemical_formula_sum            'C60 H92 O2 P2 Rb2'
_chemical_formula_weight         1078.21
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                80.831(4)
_cell_angle_beta                 83.722(4)
_cell_angle_gamma                83.847(5)
_cell_formula_units_Z            2
_cell_length_a                   13.7831(13)
_cell_length_b                   14.0866(14)
_cell_length_c                   18.4745(17)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    120
_cell_measurement_theta_max      23.904
_cell_measurement_theta_min      2.189
_cell_volume                     3505.1(6)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS, 2016)'
_computing_data_collection       'SAINT V8.40B (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS, 2016)'
_computing_molecular_graphics    'Diamond 4 (Brandenburg, 1997)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker APEX II'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.711
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_correction_T_min  0.7426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0801 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.9265.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.932
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         14299
_refine_ls_number_restraints     322
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0951P)^2^+2.0173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8488
_reflns_number_total             14299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02721c2.cif
_cod_data_source_block           bn00743
_cod_depositor_comments
'Adding full bibliography for 7717331--7717346.cif.'
_cod_database_code               7717344
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.747
_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. Restrained distances
 C19B-C25B = C19A-C25A
 1.53 with sigma of 0.02
 C25B-C26B = C25B-C27B = C25A-C26A = C25A-C27A
 1.54 with sigma of 0.02
 Rb2-C50A \\sim Rb2-C50B
 with sigma of 0.02
 C51-C50A \\sim C51-C50B
 with sigma of 0.02
 C47-C48A \\sim C47-C48B
 with sigma of 0.02
 C50A-C49A \\sim C50B-C49B
 with sigma of 0.02
 C48A-C49A \\sim C48B-C49B
 with sigma of 0.02
 C56A-C54A \\sim C56B-C54B
 with sigma of 0.02
 C49A-C54A \\sim C49B-C54B
 with sigma of 0.02
 C54A-C55A \\sim C54B-C55B
 with sigma of 0.02
 Rb2-C49A \\sim Rb2-C49B
 with sigma of 0.04
 C51-C49A \\sim C51-C49B
 with sigma of 0.04
 C47-C49A \\sim C47-C49B
 with sigma of 0.04
 C50A-C48A \\sim C50B-C48B
 with sigma of 0.04
 C50A-C54A \\sim C50B-C54B
 with sigma of 0.04
 C48A-C54A \\sim C48B-C54B
 with sigma of 0.04
 C56A-C49A \\sim C56B-C49B
 with sigma of 0.04
 C56A-C55A \\sim C56B-C55B
 with sigma of 0.04
 C49A-C55A \\sim C49B-C55B
 with sigma of 0.04
 C21-C20B \\sim C21-C20A
 with sigma of 0.02
 C17-C18B \\sim C17-C18A
 with sigma of 0.02
 C20B-C19B \\sim C20A-C19A
 with sigma of 0.02
 C18B-C19B \\sim C18A-C19A
 with sigma of 0.02
 C19B-C25B \\sim C19A-C25A
 with sigma of 0.02
 C26B-C25B \\sim C26A-C25A
 with sigma of 0.02
 C21-C19B \\sim C21-C19A
 with sigma of 0.04
 C17-C19B \\sim C17-C19A
 with sigma of 0.04
 C20B-C18B \\sim C20A-C18A
 with sigma of 0.04
 C20B-C25B \\sim C20A-C25A
 with sigma of 0.04
 C18B-C25B \\sim C18A-C25A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C49A) \\sim Ueq, Uanis(C49B) \\sim Ueq, Uanis(C50A) \\sim Ueq,
Uanis(C50B) \\sim Ueq, Uanis(C54B) \\sim Ueq, Uanis(C56B) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C55B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C26A) \\sim Ueq,
Uanis(C27A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C20A) \\sim Ueq, Uanis(C25B) \\sim Ueq, Uanis(C26B) \\sim Ueq,
Uanis(C27B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C40, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48A, C49A, C50A, C54A, C55A, C56A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48B, C49B, C50B, C54B, C55B, C56B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C17, C18B, C19B, C20B, C21, C25B, C26B, C27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C17, C18A, C19A, C20A, C21, C25A, C26A, C27A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(C20B)=Sof(H20B)=Sof(C25B)=Sof(H25B)=
 Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27B)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=1-FVAR(1)
 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C25A)=Sof(H25A)=
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=FVAR(1)
 Sof(C48B)=Sof(H48B)=Sof(C49B)=Sof(C50B)=Sof(H50B)=Sof(C54B)=Sof(H54B)=
 Sof(C55B)=Sof(H55D)=Sof(H55E)=Sof(H55F)=Sof(C56B)=Sof(H56D)=Sof(H56E)=
 Sof(H56F)=1-FVAR(2)
 Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(C50A)=Sof(H50A)=Sof(C54A)=Sof(H54A)=
 Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56A)=Sof(H56A)=Sof(H56B)=
 Sof(H56C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C22(H22), C25B(H25B), C25A(H25A), C28(H28),
 C37(H37), C40(H40), C43(H43), C52(H52), C54B(H54B), C54A(H54A), C58(H58)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C18B(H18B), C18A(H18A), C20B(H20B), C20A(H20A), C33(H33),
 C35(H35), C48A(H48A), C48B(H48B), C50A(H50A), C50B(H50B)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26B(H26A,H26B,H26C), C26A(H26D,H26E,H26F), C27A(H27A,H27B,H27C),
 C27B(H27D,H27E,H27F), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C53(H53A,H53B,H53C), C54(H54C,H54D,H54E),
 C55A(H55A,H55B,H55C), C55B(H55D,H55E,H55F), C56A(H56A,H56B,H56C), C56B(H56D,
 H56E,H56F), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40040
_shelx_hkl_checksum              37739
_shelx_fab_checksum              72174
_olex2_date_sample_data_collection 2024-07-02
_olex2_date_sample_submission    2024-07-01
_olex2_submission_special_instructions 'No special instructions were received'