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_7717331
_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         'C48 H68 Li2 O5 P2'
_chemical_formula_sum            'C48 H68 Li2 O5 P2'
_chemical_formula_weight         800.84
_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             2023-12-22
_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                105.308(4)
_cell_angle_beta                 97.164(4)
_cell_angle_gamma                91.535(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9740(14)
_cell_length_b                   11.1322(14)
_cell_length_c                   19.511(3)
_cell_measurement_reflns_used    8252
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.081
_cell_measurement_theta_min      2.185
_cell_volume                     2276.6(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 0.914
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.166
_diffrn_reflns_theta_min         1.900
_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    0.139
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0807 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.9247.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         13444
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0529P)^2^+1.1234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9115
_reflns_number_total             13444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02721c2.cif
_cod_data_source_block           bn00611
_cod_depositor_comments
'Adding full bibliography for 7717331--7717346.cif.'
_cod_database_code               7717331
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C44A \\sim O4-C44B
 with sigma of 0.02
 C42-C43A \\sim C42-C43B
 with sigma of 0.02
 C43A-C44A \\sim C43B-C44B
 with sigma of 0.02
 O4-C43A \\sim O4-C43B
 with sigma of 0.04
 C42-C44A \\sim C42-C44B
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C43A, C44A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43B, C44B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44C)=
 Sof(H44D)=1-FVAR(1)
 Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C44A)=Sof(H44A)=
 Sof(H44B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C42(H42C,H42D), C43A(H43A,H43B), C44A(H44A,H44B),
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C43B(H43C,
 H43D), C44B(H44C,H44D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23), C30(H30), C32(H32)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_shelx_res_checksum              31297
_shelx_hkl_checksum              14820
_olex2_date_sample_data_collection 2023-12-21
_olex2_date_sample_submission    2023-12-20
_olex2_submission_special_instructions 'No special instructions were received'