Cyclometalated (NNC)Ru(II) complex catalyzed β-methylation of alcohols using methanol
Ganguli, Kasturi; Belkova, Natalia; Kundu, Sabuj; Dalton Transactions  (2022) –; doi:10.1039/D1DT03967A

data_7709422
_publ_section_title
;
 Cyclometalated (NNC)Ru(II) complex catalyzed \b-methylation of alcohols
 using methanol
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03967A
_journal_year                    2022
_chemical_formula_moiety         'C57 H44 Cl N3 O P2 Ru'
_chemical_formula_sum            'C57 H44 Cl N3 O P2 Ru'
_chemical_formula_weight         985.41
_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     iterative
_audit_creation_date             2021-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.007(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9682(12)
_cell_length_b                   22.876(2)
_cell_length_c                   16.6453(15)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.29
_cell_volume                     5220.9(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            58738
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.764
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5181
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1634 before and 0.0795 after correction.
The Ratio of minimum to maximum transmission is 0.6948.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.918
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0877P)^2^+16.9399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7010
_reflns_number_total             9167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03967a2.cif
_cod_data_source_block           18sepa
_cod_original_cell_volume        5221.0(8)
_cod_database_code               7709422
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.956
_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:
 C00B(H00B), C00C(H00C), C00D(H00D), C00F(H00F), C00G(H00G), C00M(H00M),
 C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V),
 C00X(H00X), C00Y(H00Y), C010(H010), C011(H011), C013(H013), C014(H014),
 C015(H015), C016(H016), C018(H018), C019(H019), C01A(H01A), C01B(H01B),
 C01D(H01D), C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J),
 C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01U(H01U), C01V(H01V)
2.b Idealised Me refined as rotating group:
 C01Y(H01C,H01E,H01T)
;
_shelx_res_checksum              69171
_shelx_fab_checksum              94653
_olex2_submission_special_instructions 'No special instructions were received'