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_7717339
_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         'C72 H88 Cs4 O4 P4, 0.5(C6 H14)'
_chemical_formula_sum            'C75 H95 Cs4 O4 P4'
_chemical_formula_weight         1716.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-25
_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                 127.598(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.406(7)
_cell_length_b                   20.260(4)
_cell_length_c                   28.672(5)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.202
_cell_measurement_theta_min      2.317
_cell_volume                     16296(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            106530
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.050
_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    1.896
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0586 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.8955.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       plank
_exptl_crystal_F_000             6856
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.483
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         20200
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0561P)^2^+56.6870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13750
_reflns_number_total             20200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02721c2.cif
_cod_data_source_block           bn00506_0m
_cod_depositor_comments
'Adding full bibliography for 7717331--7717346.cif.'
_cod_original_cell_volume        16295(5)
_cod_database_code               7717339
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.848
_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
 P1-C10B \\sim P1-C10A
 with sigma of 0.02
 C10B-C11B \\sim C10A-C11A
 with sigma of 0.02
 C10B-C15B \\sim C10A-C15A
 with sigma of 0.02
 C11B-C12B \\sim C11A-C12A
 with sigma of 0.02
 C11B-C16B \\sim C11A-C16A
 with sigma of 0.02
 C12B-C13B \\sim C12A-C13A
 with sigma of 0.02
 C13B-C14B \\sim C13A-C14A
 with sigma of 0.02
 C13B-C17B \\sim C13A-C17A
 with sigma of 0.02
 C14B-C15B \\sim C14A-C15A
 with sigma of 0.02
 C15B-C18B \\sim C15A-C18A
 with sigma of 0.02
 P1-C11B \\sim P1-C11A
 with sigma of 0.04
 P1-C15B \\sim P1-C15A
 with sigma of 0.04
 C10B-C12B \\sim C10A-C12A
 with sigma of 0.04
 C10B-C14B \\sim C10A-C14A
 with sigma of 0.04
 C10B-C16B \\sim C10A-C16A
 with sigma of 0.04
 C10B-C18B \\sim C10A-C18A
 with sigma of 0.04
 C11B-C13B \\sim C11A-C13A
 with sigma of 0.04
 C11B-C15B \\sim C11A-C15A
 with sigma of 0.04
 C12B-C14B \\sim C12A-C14A
 with sigma of 0.04
 C12B-C16B \\sim C12A-C16A
 with sigma of 0.04
 C12B-C17B \\sim C12A-C17A
 with sigma of 0.04
 C13B-C15B \\sim C13A-C15A
 with sigma of 0.04
 C14B-C17B \\sim C14A-C17A
 with sigma of 0.04
 C14B-C18B \\sim C14A-C18A
 with sigma of 0.04
 C73A-C74A \\sim C73B-C74B
 with sigma of 0.02
 C74A-C75A \\sim C74B-C75B
 with sigma of 0.02
 C75A-C75A_$1 \\sim C75B-C75B_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10A) \\sim Ueq, Uanis(C11A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C12B) \\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C73B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C73A) \\sim Ueq, Uanis(C74B) \\sim Ueq, Uanis(C75B) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C10B, C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C10B)=Sof(C11B)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(C14B)=Sof(H14B)=
 Sof(C15B)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17B)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C10A)=Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=
 Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17A)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
 Sof(C73B)=Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(C74B)=Sof(H74C)=Sof(H74D)=
 Sof(C75B)=Sof(H75C)=Sof(H75D)=1-FVAR(2)
 Sof(C73A)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C74A)=Sof(H74A)=Sof(H74B)=
 Sof(C75A)=Sof(H75A)=Sof(H75B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C74A(H74A,H74B), C74B(H74C,H74D), C75A(H75A,H75B), C75B(H75C,H75D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12A(H12A), C12B(H12B), C14A(H14A), C14B(H14B), C21(H21),
 C23(H23), C30(H30), C32(H32), C39(H39), C41(H41), C48(H48), C50(H50), C57(H57),
  C59(H59), C66(H66), C68(H68)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16A(H16A,H16B,H16C),
 C16B(H16D,H16E,H16F), C17A(H17A,H17B,H17C), C17B(H17D,H17E,H17F), C18A(H18A,
 H18B,H18C), C18B(H18D,H18E,H18F), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C52(H52A,
 H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C70(H70A,H70B,H70C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C), C73A(H73A,H73B,H73C), C73B(H73D,H73E,H73F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23
_shelx_hkl_checksum              10864
_shelx_fab_checksum              27089
_olex2_submission_special_instructions 'No special instructions were received'