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_7709421
_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         'C56 H42 Cl N3 P2 Ru'
_chemical_formula_sum            'C56 H42 Cl N3 P2 Ru'
_chemical_formula_weight         955.38
_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     dual
_audit_creation_date             2021-04-02
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.647(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.390(2)
_cell_length_b                   22.927(4)
_cell_length_c                   16.646(3)
_cell_measurement_reflns_used    7336
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.328
_cell_measurement_theta_min      2.636
_cell_volume                     5037.9(15)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1430
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            75666
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.636
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       prism
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         12498
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+5.2220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7336
_reflns_number_total             12498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03967a2.cif
_cod_data_source_block           20jana_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        5038.0(14)
_cod_database_code               7709421
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C39: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C44, C43, C42, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C38(H38), C15(H15), C29(H29), C18(H18), C20(H20), C50(H50),
 C5(H5), C28(H28), C56(H56), C46(H46), C14(H14), C48(H48), C9(H9), C49(H49),
 C17(H17), C11(H11), C10(H10), C2(H2), C47(H47), C35(H35), C16(H16), C37(H37),
 C4(H4), C12(H12), C54(H54), C34(H34), C3(H3), C25(H25), C36(H36), C24(H24),
 C55(H55), C22(H22), C52(H52), C53(H53), C23(H23), C44(H44), C43(H43), C42(H42),
  C41(H41), C40(H40)
4.b Fitted hexagon refined as free rotating group:
 C44(C43,C42,C41,C40,C39)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2529
_shelx_fab_checksum              34431
_olex2_submission_special_instructions 'No special instructions were received'