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_7717346
_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         'C102 H174 K8 N4 O7 P4 Si8'
_chemical_formula_sum            'C102 H174 K8 N4 O7 P4 Si8'
_chemical_formula_weight         2229.84
_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             2023-04-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.933(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4093(15)
_cell_length_b                   62.066(8)
_cell_length_c                   17.263(2)
_cell_measurement_reflns_used    9012
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.161
_cell_measurement_theta_min      2.234
_cell_volume                     12785(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0561
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       74
_diffrn_reflns_limit_k_min       -74
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            80690
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.797
_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    0.441
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.7914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1009 before and 0.0635 after correction.
The Ratio of minimum to maximum transmission is 0.8258.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       prism
_exptl_crystal_F_000             4776
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1401
_refine_ls_number_reflns         23136
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0854
_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^)+67.4268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16167
_reflns_number_total             23136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02721c2.cif
_cod_data_source_block           bn00476_0m
_cod_depositor_comments
'Adding full bibliography for 7717331--7717346.cif.'
_cod_database_code               7717346
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.909
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2-C4A \\sim Si2-C4B
 with sigma of 0.02
 Si2-C5A \\sim Si2-C5B
 with sigma of 0.02
 Si2-C6A \\sim Si2-C6B
 with sigma of 0.02
 P4-C79B \\sim P4-C79A
 with sigma of 0.02
 C79B-C80B \\sim C79A-C80A
 with sigma of 0.02
 C79B-C84B \\sim C79A-C84A
 with sigma of 0.02
 C80B-C81B \\sim C80A-C81A
 with sigma of 0.02
 C80B-C85B \\sim C80A-C85A
 with sigma of 0.02
 C81B-C82B \\sim C81A-C82A
 with sigma of 0.02
 C82B-C83B \\sim C82A-C83A
 with sigma of 0.02
 C82B-C86B \\sim C82A-C86A
 with sigma of 0.02
 C83B-C84B \\sim C83A-C84A
 with sigma of 0.02
 C84B-C87B \\sim C84A-C87A
 with sigma of 0.02
 K6-C79B \\sim K6-C79A
 with sigma of 0.04
 K6-C80B \\sim K6-C80A
 with sigma of 0.04
 K6-C81B \\sim K6-C81A
 with sigma of 0.04
 K6-C84B \\sim K6-C84A
 with sigma of 0.04
 K6-C85B \\sim K6-C85A
 with sigma of 0.04
 P4-C80B \\sim P4-C80A
 with sigma of 0.04
 P4-C84B \\sim P4-C84A
 with sigma of 0.04
 C79B-C81B \\sim C79A-C81A
 with sigma of 0.04
 C79B-C83B \\sim C79A-C83A
 with sigma of 0.04
 C79B-C85B \\sim C79A-C85A
 with sigma of 0.04
 C79B-C87B \\sim C79A-C87A
 with sigma of 0.04
 C80B-C82B \\sim C80A-C82A
 with sigma of 0.04
 C80B-C84B \\sim C80A-C84A
 with sigma of 0.04
 C81B-C83B \\sim C81A-C83A
 with sigma of 0.04
 C81B-C85B \\sim C81A-C85A
 with sigma of 0.04
 C81B-C86B \\sim C81A-C86A
 with sigma of 0.04
 C82B-C84B \\sim C82A-C84A
 with sigma of 0.04
 C83B-C86B \\sim C83A-C86A
 with sigma of 0.04
 C83B-C87B \\sim C83A-C87A
 with sigma of 0.04
 O6-C0A \\sim O6-C0B
 with sigma of 0.02
 C0A-C1A \\sim C0B-C1B
 with sigma of 0.02
 C1A-O7A \\sim C1B-O7B
 with sigma of 0.02
 O7A-C2A \\sim O7B-C2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C80A) \\sim Ueq, Uanis(C81A) \\sim Ueq, Uanis(C82A) \\sim Ueq,
Uanis(C83A) \\sim Ueq, Uanis(C84A) \\sim Ueq, Uanis(C85A) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C79B) \\sim Ueq, Uanis(C85B) \\sim Ueq, Uanis(C87B) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C79A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C79B, C80B, C81B, C82B, C83B, C84B, C85B, C86B, C87B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C79A, C80A, C81A, C82A, C83A, C84A, C85A, C86A, C87A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O6, O7A, C0A, C1A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, O7B, C0B, C1B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O7B)=Sof(C0B)=Sof(H0BA)=Sof(H0BB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=
 Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=Sof(C5B)=
 Sof(H5BA)=Sof(H5BB)=Sof(H5BC)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=1-FVAR(1)
 Sof(O7A)=Sof(C0A)=Sof(H0AA)=Sof(H0AB)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=
 Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=FVAR(1)
 Sof(C79A)=Sof(C80A)=Sof(C81A)=Sof(H81A)=Sof(C82A)=Sof(C83A)=Sof(H83A)=
 Sof(C84A)=Sof(C85A)=Sof(H85A)=Sof(H85B)=Sof(H85C)=Sof(C86A)=Sof(H86A)=
 Sof(H86B)=Sof(H86C)=Sof(C87A)=Sof(H87A)=Sof(H87B)=Sof(H87C)=1-FVAR(2)
 Sof(C79B)=Sof(C80B)=Sof(C81B)=Sof(H81B)=Sof(C82B)=Sof(C83B)=Sof(H83B)=
 Sof(C84B)=Sof(C85B)=Sof(H85D)=Sof(H85E)=Sof(H85F)=Sof(C86B)=Sof(H86D)=
 Sof(H86E)=Sof(H86F)=Sof(C87B)=Sof(H87D)=Sof(H87E)=Sof(H87F)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C0A(H0AA,H0AB), C0B(H0BA,H0BB), C1A(H1AA,H1AB), C1B(H1BA,H1BB), C98(H98A,
 H98B), C99(H99A,H99B)
6.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C36(H36), C38(H38), C45(H45), C47(H47), C54(H54),
 C56(H56), C63(H63), C65(H65), C72(H72), C74(H74), C81A(H81A), C81B(H81B),
 C83A(H83A), C83B(H83B), C90(H90), C92(H92)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC),
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC), C4B(H4BA,H4BB,H4BC),
 C5A(H5AA,H5AB,H5AC), C5B(H5BA,H5BB,H5BC), C6A(H6AA,H6AB,H6AC), C6B(H6BA,H6BB,
 H6BC), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C76(H76A,H76B,H76C),
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C85A(H85A,H85B,H85C), C85B(H85D,H85E,
 H85F), C86A(H86A,H86B,H86C), C86B(H86D,H86E,H86F), C87A(H87A,H87B,H87C),
 C87B(H87D,H87E,H87F), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,
 H96C), C97(H97A,H97B,H97C)
;
_shelx_res_checksum              13827
_shelx_hkl_checksum              41969
_olex2_date_sample_data_collection 2023-04-25
_olex2_date_sample_submission    2023-04-21
_olex2_submission_special_instructions 'No special instructions were received'