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_7716296
_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         'C41 H41 Cl2 N P2 Ru'
_chemical_formula_sum            'C41 H41 Cl2 N P2 Ru'
_chemical_formula_weight         781.66
_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     iterative
_audit_creation_date             2024-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-22 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7777(2)
_cell_length_b                   11.30550(10)
_cell_length_c                   17.3485(2)
_cell_measurement_reflns_used    21486
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.5200
_cell_measurement_theta_min      2.1100
_cell_volume                     3619.47(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f     25.73 209.23   0.50    2.00  75.04 -15.82  31.50    --   367
  2  \w   -115.72  16.28   0.50    2.00    --  -15.82 -59.25 173.08  264
  3  \w   -115.72  16.28   0.50    2.00    --  -15.82 -59.25  20.08  264
  4  \w   -115.72  16.28   0.50    2.00    --  -15.82 -59.25 122.08  264
  5  \f    -49.73 133.77   0.50    2.00  13.01 -15.82 -31.50    --   367
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0150655000
_diffrn_orient_matrix_UB_12      0.0544847000
_diffrn_orient_matrix_UB_13      0.0153492000
_diffrn_orient_matrix_UB_21      -0.0194556000
_diffrn_orient_matrix_UB_22      0.0299758000
_diffrn_orient_matrix_UB_23      -0.0332469000
_diffrn_orient_matrix_UB_31      -0.0295229000
_diffrn_orient_matrix_UB_32      0.0080854000
_diffrn_orient_matrix_UB_33      0.0197765000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82029
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.207
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         10519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0405P)^2^+2.9918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8791
_reflns_number_total             10519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00940a2.cif
_cod_data_source_block           compound_7
_cod_depositor_comments
'Adding full bibliography for 7716295--7716298.cif.'
_cod_database_code               7716296
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C39(H39)
1.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
1.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C38(H38), C37(H37), C35(H35), C25(H25), C31(H31), C34(H34), C3(H3),
 C27(H27), C12(H12), C21(H21), C2(H2), C28(H28), C16(H16), C8(H8), C17(H17),
 C24(H24), C29(H29), C15(H15), C30(H30), C9(H9), C23(H23), C14(H14), C11(H11),
 C10(H10), C4(H4), C6(H6), C5(H5), C22(H22)
1.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.392
_oxdiff_exptl_absorpt_empirical_full_min 0.272