Arene displacement, C-H activation and acetonitrile insertion reactions enabled by coordination of a functionalized iminophosphorane to a Ru<sup>II</sup>-<i>p</i>-cymene scaffold.
Gourkhede, Rani; Kaur, Bhupinder; Kote, Basvaraj S.; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10693–10703; doi:10.1039/d4dt00940a

data_7716297
_publ_section_title
;
 Arene displacement, C-H activation and acetonitrile insertion reactions
 enabled by coordination of a functionalized iminophosphorane to a
 Ru<sup>II</sup>-<i>p</i>-cymene scaffold.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10693
_journal_page_last               10703
_journal_paper_doi               10.1039/d4dt00940a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C58 H48 Cl N O P2 Ru, 0.718(C H2 Cl2), 0.5[CH2Cl2]'
_chemical_formula_sum            'C59.218 H50.435 Cl3.435 N O P2 Ru'
_chemical_formula_weight         1076.909
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2024-05-21
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.05.15 svn.r971b711c for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-05-22 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.198(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4145(8)
_cell_length_b                   15.8158(8)
_cell_length_c                   23.9074(13)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      27.394
_cell_measurement_theta_min      2.245
_cell_volume                     5327.3(5)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.00
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1364
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            123416
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9993
_diffrn_reflns_theta_full        24.9991
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5848
_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            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             2211.265
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.9715
_refine_diff_density_min         -0.5962
_refine_diff_density_rms         0.0980
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             11.0752
_refine_ls_extinction_coef       0.00044(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    97
_refine_ls_number_parameters     606
_refine_ls_number_reflns         9368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0877
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+7.0268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              -12
_reflns_number_gt                6661
_reflns_number_total             9368
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00940a2.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
'Adding full bibliography for 7716295--7716298.cif.'
_cod_original_formula_sum        'C59.218 H50.435 Cl3.435 N1 O1 P2 Ru1'
_cod_database_code               7716297
_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. Others
 Sof(C59)=Sof(H59a)=Sof(H59b)=Sof(Cl3)=Sof(Cl2)=Sof(H59a)=Sof(H59b)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C8(H8), C21(H21)
3.b Secondary CH2 refined with riding coordinates:
 C46(H46a,H46b), C59(H59a,H59b)
3.c Me refined with riding coordinates:
 C7(H7b,H7a,H7c)
3.d Aromatic/amide H refined with riding coordinates:
 C36(H36), C37(H37), C38(H38), C39(H39), C33(H33), C32(H32), C31(H31),
 C30(H30), C29(H29), C5(H5), C3(H3), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C27(H27), C26(H26), C25(H25), C24(H24), C23(H23), C58(H58), C57(H57),
  C56(H56), C55(H55), C54(H54), C48(H48), C49(H49), C50(H50), C51(H51),
 C52(H52), C20(H20), C19(H19), C18(H18), C17(H17), C16(H16), C10(H10), C11(H11),
  C12(H12), C13(H13), C14(H14)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'