A novel access to phosphanylidene-phosphorane complexes via P-donor substitution and a detailed bonding analysis
Biskup, David; Schnakenburg, Gregor; Boeré, René; Espinosa Ferao, Arturo; Streubel, R.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02304D

data_7713946
_publ_section_title
;
 A novel access to phosphanylidene-phosphorane complexes via P-donor
 substitution and a detailed bonding analysis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02304D
_journal_year                    2023
_chemical_formula_moiety         'C27 H24 Cr O5 P2'
_chemical_formula_sum            'C27 H24 Cr O5 P2'
_chemical_formula_weight         542.42
_chemical_name_systematic        DB-565
_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
_audit_creation_date             2022-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                88.1908(19)
_cell_angle_beta                 76.3409(17)
_cell_angle_gamma                70.2330(18)
_cell_formula_units_Z            2
_cell_length_a                   9.06234(20)
_cell_length_b                   9.31754(23)
_cell_length_c                   15.9532(3)
_cell_measurement_reflns_used    36831
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.02
_cell_measurement_theta_min      5.05
_cell_volume                     1230.12(5)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)'
_computing_data_reduction
'X-Area Integrate 2.5.1.0 (STOE, 2021) X-Area LANA 2.6.2.0 (STOE, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24426
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.525
_diffrn_reflns_theta_min         5.051
_diffrn_source                   'Axo Cu'
_exptl_absorpt_coefficient_mu    5.38
_exptl_absorpt_correction_T_max  0.2633
_exptl_absorpt_correction_T_min  0.1558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'STOE X-Red32, absorption correction by Gaussian integration, analogous to P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. Finally a spherical absorption correction was done within STOE LANA.'
_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    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.058
_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     319
_refine_ls_number_reflns         4602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0462P)^2^+0.8953P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4485
_reflns_number_total             4602
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d3dt02304d2.cif
_cod_data_source_block           3a-Cr
_cod_database_code               7713946
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.673
_shelx_estimated_absorpt_t_min   0.296
_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:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              41361
_olex2_submission_special_instructions 'No special instructions were received'