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_7717345
_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         'C54 H90 K2 N6 O2 P2'
_chemical_formula_sum            'C54 H90 K2 N6 O2 P2'
_chemical_formula_weight         995.45
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.428(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1372(2)
_cell_length_b                   19.6662(3)
_cell_length_c                   12.7854(2)
_cell_measurement_reflns_used    23235
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.480
_cell_measurement_theta_min      2.043
_cell_volume                     2927.19(8)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi + omega - scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23235
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.043
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.673
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_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+1.7318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6026
_reflns_number_total             6699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02721c2.cif
_cod_data_source_block           FO7187
_cod_depositor_comments
'Adding full bibliography for 7717331--7717346.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717345
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              4336
_shelx_hkl_checksum              82404