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_7717342
_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         'C90 H139 Cs2 O3 P3'
_chemical_formula_sum            'C90 H139 Cs2 O3 P3'
_chemical_formula_weight         1627.73
_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     dual
_audit_creation_date             2024-07-12
_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                72.089(3)
_cell_angle_beta                 62.708(3)
_cell_angle_gamma                81.454(3)
_cell_formula_units_Z            2
_cell_length_a                   18.486(2)
_cell_length_b                   18.651(2)
_cell_length_c                   19.470(2)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.711
_cell_measurement_theta_min      2.223
_cell_volume                     5676.3(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0772
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62243
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.083
_diffrn_reflns_theta_max         25.083
_diffrn_reflns_theta_min         1.240
_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    0.719
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1061 before and 0.0818 after correction.
The Ratio of minimum to maximum transmission is 0.8589.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.952
_exptl_crystal_description       prism
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.993
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         20031
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0734
_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^)+(0.0969P)^2^+23.0230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.2262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11317
_reflns_number_total             20031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02721c2.cif
_cod_data_source_block           bn00758
_cod_depositor_comments
'Adding full bibliography for 7717331--7717346.cif.'
_cod_original_cell_volume        5676.1(12)
_cod_database_code               7717342
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 P3-H3
 1.3 with sigma of 0.02
 C88-C90A \\sim C88-C90B
 with sigma of 0.02
 C49-C55A \\sim C49-C55B
 with sigma of 0.02
 C57-C55A \\sim C57-C55B
 with sigma of 0.02
 C55A-C56A \\sim C55B-C56B
 with sigma of 0.02
 C49-C56A \\sim C49-C56B
 with sigma of 0.04
 C57-C56A \\sim C57-C56B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C90B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C90A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C76) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C55A, C56A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55B, C56B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C76, C77, C78, C79, C80, C81
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C90B)=Sof(H90D)=Sof(H90E)=Sof(H90F)=1-FVAR(1)
 Sof(C90A)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(1)
 Sof(C55B)=Sof(H55B)=Sof(C56B)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(H57D)=
 Sof(H57E)=Sof(H57F)=1-FVAR(2)
 Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(H57A)=
 Sof(H57B)=Sof(H57C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C22(H22), C25(H25), C28(H28), C37(H37), C40(H40),
 C43(H43), C52(H52), C55B(H55B), C55A(H55A), C58(H58), C67(H67), C70(H70),
 C73(H73), C82(H82), C85(H85), C88(H88)
6.b Me refined with riding coordinates:
 C90A(H90A,H90B,H90C), C90B(H90D,H90E,H90F)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C18(H18), C20(H20), C33(H33), C35(H35), C48(H48), C50(H50),
 C63(H63), C65(H65), C78(H78), C80(H80)
6.d 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), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), 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(H54A,H54B,H54C), C56A(H56A,H56B,H56C), C56B(H56D,H56E,H56F),
 C57(H57A,H57B,H57C), C57(H57D,H57E,H57F), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C89(H89A,H89B,
 H89C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60818
_shelx_hkl_checksum              9875
_shelx_fab_checksum              38974
_olex2_date_sample_data_collection 2024-07-10
_olex2_date_sample_submission    2024-07-08
_olex2_submission_special_instructions 'No special instructions were received'