Highly selective, reversible water activation by P,N-cooperativity in pyridyl-functionalized phosphinines.
Kopp, Richard O.; Kleynemeyer, Sabrina L.; Groth, Lucie J.; Ernst, Moritz J.; Rupf, Susanne M.; Weber, Manuela; Kershaw Cook, Laurence J.; Coles, Nathan T.; Neale, Samuel E.; Müller, Christian; Chemical science 15 (2024) 5496–5506; doi:10.1039/d3sc05930h

data_1571250
_publ_section_title
;
 Highly selective, reversible water activation by P,N-cooperativity in
 pyridyl-functionalized phosphinines.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              5496
_journal_page_last               5506
_journal_paper_doi               10.1039/d3sc05930h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C25 H17 N4 P'
_chemical_formula_sum            'C25 H17 N4 P'
_chemical_formula_weight         404.39
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-31 deposited with the CCDC.	2024-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2936(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.0233(2)
_cell_length_b                   7.6255(2)
_cell_length_c                   21.2045(6)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.84
_cell_volume                     972.33(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Photon CMOS Detector, D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25237
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.510
_diffrn_reflns_theta_min         2.839
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_correction_T_min  0.9367
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1385 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.9407.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       Block
_exptl_crystal_F_000             420
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.272
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+1.0450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2936
_reflns_number_total             2955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05930h2.cif
_cod_data_source_block           lg012
_cod_depositor_comments
'Adding full bibliography for 1571249--1571254.cif.'
_cod_database_code               1571250
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C4) = Uanis(C5)
3. Others
 Fixed Sof: P1(0.5) C5(0.5) C1(0.5) C4(0.5) C3(0.5) H3(0.5) C2(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C7(H7), C14(H14), C8(H8), C10(H10), C13(H13), C9(H9),
 C3(H3)
;
_shelx_res_checksum              55148
_olex2_submission_special_instructions 'No special instructions were received'