Photoswitchable Electron-rich Phosphines: Using Light to Modulate the Electron-Donating Ability of Phosphines
Buß, Florenz; Das, Mowpriya; Janssen-Mueller, Daniel; Sietmann, Alexander; Das, Ankita; Wilm, Lukas F. B.; Freitag, Matthias; Seidl, Michael; Glorius, Frank; Dielmann, Fabian; Chemical Communications  (2023) –; doi:10.1039/D3CC04050J

data_7132121
_publ_section_title
;
 Photoswitchable Electron-rich Phosphines: Using Light to Modulate the
 Electron-Donating Ability of Phosphines
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04050J
_journal_year                    2023
_chemical_formula_moiety         '2(C38 H42 N3 Ni O3 P S2), C5 H12'
_chemical_formula_sum            'C81 H96 N6 Ni2 O6 P2 S4'
_chemical_formula_weight         1557.23
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-10
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6811)
;
_audit_update_record
;
2023-08-17 deposited with the CCDC.	2023-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.5820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6213(5)
_cell_length_b                   17.5686(6)
_cell_length_c                   17.6681(5)
_cell_measurement_reflns_used    9642
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.32
_cell_volume                     3931.7(2)
_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      150.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            88253
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.158
_diffrn_reflns_theta_min         1.982
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0736 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.9416.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8721
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0417P)^2^+2.4492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7331
_reflns_number_total             8721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04050j2.cif
_cod_data_source_block           fd23_68_0m
_cod_database_code               7132121
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_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. Uiso/Uaniso restraints and constraints
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43: within 1.9A with sigma of 0.01 and
sigma for terminal atoms of 0.01 within 1.9A
3. Others
 Fixed Sof: C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) C41(0.5) H41A(0.5) H41B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C39(0.5)
 H39A(0.5) H39B(0.5) H39C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C41(H41A,H41B), C40(H40A,H40B)
4.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C7(H7), C12(H12), C16(H16), C13(H13), C14(H14), C15(H15), C27(H27),
 C23(H23), C25(H25), C24(H24), C26(H26)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C21(H21A,H21B,H21C), C10(H10A,H10B,H10C), C30(H30A,H30B,
 H30C), C4(H4A,H4B,H4C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C31(H31A,
 H31B,H31C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C43(H43A,H43B,H43C),
 C39(H39A,H39B,H39C)
;
_shelx_res_checksum              44076
_shelx_hkl_checksum              32125
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems, Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'