Ligand controlled switchable selectivity in ruthenium catalyzed aerobic oxidation of primary amines.
Ray, Ritwika; Chandra, Shubhadeep; Yadav, Vishal; Mondal, Prasenjit; Maiti, Debabrata; Lahiri, Goutam Kumar; Chemical communications (Cambridge, England) 53 (2017) 4006–; doi:10.1039/c6cc10200j

data_7119848
_publ_section_title
;
 Ligand controlled switchable selectivity in ruthenium catalyzed aerobic
 oxidation of primary amines.
;
_journal_issue                   28
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4006
_journal_paper_doi               10.1039/c6cc10200j
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C63 H51 N2 O P2 Ru, Cl O4, 2(C H2 Cl2)'
_chemical_formula_sum            'C65 H55 Cl5 N2 O5 P2 Ru'
_chemical_formula_weight         1284.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-09 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                98.289(2)
_cell_angle_beta                 105.598(3)
_cell_angle_gamma                90.117(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8945(19)
_cell_length_b                   14.063(2)
_cell_length_c                   18.356(3)
_cell_measurement_reflns_used    23302
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      2.8
_cell_volume                     2923.8(8)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_data_reduction
'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1237
_diffrn_reflns_av_unetI/netI     0.2205
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23302
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.048
_exptl_absorpt_coefficient_mu    0.604
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.655
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         10176
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0738
_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^)+(0.0457P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5739
_reflns_number_total             10176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc10200j2.cif
_cod_data_source_block           1b_ClO4
_cod_depositor_comments
'Adding full bibliography for 7119847--7119849.cif.'
_cod_database_code               7119848
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.794
_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. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C64) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N2) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C65(H65A,H65B)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C62(H62), C59(H59), C24(H24), C3(H3), C57(H57), C17(H17), C14(H14),
 C7(H7), C23(H23), C63(H63), C60(H60), C8(H8), C15(H15), C45(H45), C53(H53),
 C61(H61), C41(H41), C21(H21), C20(H20), C51(H51), C9(H9), C29(H29), C42(H42),
 C47(H47), C44(H44), C56(H56), C38(H38), C50(H50), C33(H33), C35(H35), C39(H39),
  C43(H43), C4(H4), C54(H54), C48(H48), C5(H5), C55(H55), C30(H30), C37(H37),
 C36(H36), C49(H49), C31(H31), C32(H32)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              26815
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'