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_7716298
_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         'C66 H61 N5 P2 Ru, 1.6(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C67.6 H64.2 B2 Cl3.2 F8 N5 P2 Ru'
_chemical_formula_weight         1396.793
_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'
_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                 99.495(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.422(4)
_cell_length_b                   21.209(5)
_cell_length_c                   24.410(7)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.30
_cell_volume                     6854(3)
_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      150.00
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1602
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.9995
_diffrn_reflns_Laue_measured_fraction_max 0.9995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            155476
_diffrn_reflns_point_group_measured_fraction_full 0.9995
_diffrn_reflns_point_group_measured_fraction_max 0.9995
_diffrn_reflns_theta_full        24.9998
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.6572
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1440 before and 0.1190 after correction.
The Ratio of minimum to maximum transmission is 0.8795.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             2860.273
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.7060
_refine_diff_density_min         -0.6274
_refine_diff_density_rms         0.1035
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             10.7714
_refine_ls_goodness_of_fit_ref   1.0572
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    117
_refine_ls_number_parameters     861
_refine_ls_number_reflns         12061
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.0523
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+5.3153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                9478
_reflns_number_total             12061
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00940a2.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
'Adding full bibliography for 7716295--7716298.cif.'
_cod_database_code               7716298
_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. Restrained distances
 F1-B1 \\sim F1a-B1a
 with sigma of 0.02
 F3-B1 \\sim F3a-B1a
 with sigma of 0.02
 F2-B1 \\sim F2a-B1a
 with sigma of 0.02
 F4-B1 \\sim F4a-B1a
 with sigma of 0.02
 F1-F3 \\sim F1a-F3a
 with sigma of 0.04
 F1-F2 \\sim F1a-F2a
 with sigma of 0.04
 F1-F4 \\sim F1a-F4a
 with sigma of 0.04
 F3-F2 \\sim F3a-F2a
 with sigma of 0.04
 F3-F4 \\sim F3a-F4a
 with sigma of 0.04
 F2-F4 \\sim F2a-F4a
 with sigma of 0.04
 F1a-F3a \\sim F1a-F2a \\sim F1a-F4a \\sim F3a-F2a \\sim F3a-F4a \\sim F2a-F4a
 with sigma of 0.002
 B1a-F1a \\sim B1a-F3a \\sim B1a-F2a \\sim B1a-F4a
 with sigma of 0.001
 F1-F3 \\sim F1-F2 \\sim F1-F4 \\sim F3-F2 \\sim F3-F4 \\sim F2-F4
 with sigma of 0.002
 B1-F1 \\sim B1-F3 \\sim B1-F2 \\sim B1-F4
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
B1 \\sim B1a: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Rigid body (RIGU) restrains
 F1a, B1a, F3a, F2a, F4a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2, F1, B1, F3, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl4(0.8) Cl3(0.8) F1(0.8) Cl1(0.8) Cl2(0.8) F3(0.8) F2(0.8)
 F4(0.8) C68(0.8) H68a(0.8) H68b(0.8) B1(0.8) C67(0.8) H67a(0.8) H67b(0.8)
 B1a(0.2) F1a(0.2) F3a(0.2) F2a(0.2) F4a(0.2)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C21(H21)
6.b Secondary CH2 refined with riding coordinates:
 C48(H48a,H48b), C68(H68a,H68b), C67(H67a,H67b)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C33(H33), C32(H32), C31(H31), C30(H30),
  C29(H29), C27(H27), C26(H26), C25(H25), C24(H24), C23(H23), C54(H54),
 C53(H53), C52(H52), C51(H51), C50(H50), C60(H60), C59(H59), C58(H58), C57(H57),
  C56(H56), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C47(H47),
 C46(H46), C45(H45), C44(H44), C43(H43)
6.d Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C35(H35a,H35b,H35c), C64(H64a,H64b,H64c), C66(H66a,H66b,
 H66c), C62(H62a,H62b,H62c)
;
_olex2_submission_special_instructions 'No special instructions were received'