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_7717341
_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         '0.5(C144 H176 K8 O8 P8) [+ solvent]'
_chemical_formula_sum            'C72 H88 K4 O4 P4'
_chemical_formula_weight         1297.70
_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             2024-02-02
_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                115.909(2)
_cell_angle_beta                 100.464(3)
_cell_angle_gamma                94.920(3)
_cell_formula_units_Z            4
_cell_length_a                   15.6316(15)
_cell_length_b                   22.909(2)
_cell_length_c                   24.137(2)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      2.41
_cell_volume                     7511.1(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            146979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.572
_diffrn_reflns_theta_min         1.654
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.7144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0752 before and 0.0420 after correction.
The Ratio of minimum to maximum transmission is 0.9569.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       prism
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1561
_refine_ls_number_reflns         54325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0662P)^2^+3.0186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37345
_reflns_number_total             54325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02721c2.cif
_cod_data_source_block           bn00021_0m
_cod_depositor_comments
'Adding full bibliography for 7717331--7717346.cif.'
_cod_database_code               7717341
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.927
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23), C30(H30), C32(H32),
 C39(H39), C41(H41), C48(H48), C50(H50), C57(H57), C59(H59), C66(H66), C68(H68),
  C75(H75), C77(H77), C84(H84), C86(H86), C93(H93), C95(H95), C102(H102),
 C104(H104), C111(H111), C113(H113), C120(H120), C122(H122), C129(H129),
 C131(H131), C138(H138), C140(H140)
2.b 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), 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), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C),
 C81(H81A,H81B,H81C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,
 H90C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C),
 C106(H10A,H10B,H10C), C107(H10D,H10E,H10F), C108(H10G,H10H,H10I), C115(H11A,
 H11B,H11C), C116(H11D,H11E,H11F), C117(H11G,H11H,H11I), C124(H12A,H12B,H12C),
 C125(H12D,H12E,H12F), C126(H12G,H12H,H12I), C133(H13A,H13B,H13C), C134(H13D,
 H13E,H13F), C135(H13G,H13H,H13I), C142(H14A,H14B,H14C), C143(H14D,H14E,H14F),
 C144(H14G,H14H,H14I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3194
_shelx_hkl_checksum              64676
_shelx_fab_checksum              75927
_olex2_date_sample_data_collection 2021-09-30
_olex2_date_sample_submission    2021-09-30
_olex2_submission_original_sample_id BF-524
_olex2_submission_special_instructions 'No special instructions were received'