ortho-Amino group functionalized 2,2′-bipyridine based Ru(ii) complex catalysed alkylation of secondary alcohols, nitriles and amines using alcohols
Roy, Bivas Chandra; Debnath, Subhankar; Chakrabarti, Kaushik; Paul, Bhaskar; Maji, Milan; Kundu, Sabuj; Organic Chemistry Frontiers 5 (2018) 1008–; doi:10.1039/C7QO01061C

data_1553962
_publ_section_title
;
 ortho-Amino group functionalized 2,2&#x2032;-bipyridine based Ru(ii)
 complex catalysed alkylation of secondary alcohols, nitriles and amines
 using alcohols
;
_journal_issue                   6
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1008
_journal_paper_doi               10.1039/C7QO01061C
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C48 H44 Cl2 N4 P2 Ru'
_chemical_formula_sum            'C48 H44 Cl2 N4 P2 Ru'
_chemical_formula_weight         910.78
_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     dual
_audit_creation_date             2017-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-08-10 deposited with the CCDC.
2018-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.489(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.679(3)
_cell_length_b                   19.168(6)
_cell_length_c                   21.719(7)
_cell_measurement_reflns_used    1825
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      2.32
_cell_volume                     4028(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0955
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21149
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.112
_diffrn_reflns_theta_max         25.112
_diffrn_reflns_theta_min         1.417
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6789
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0643 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.9110.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.027
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0606
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4185
_reflns_number_total             7149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qo01061c2.cif
_cod_data_source_block           complex1b
_cod_database_code               1553962
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1), C50(H50), C46(H46), C49(H49), C30(H30), C24(H24), C32(H32),
 C43(H43), C14(H14), C41(H41), C18(H18), C47(H47), C27(H27), C40(H40), C35(H35),
  C26(H26), C42(H42), C23(H23), C22(H22), C16(H16), C20(H20), C17(H17),
 C33(H33), C39(H39), C28(H28), C29(H29), C10(H10), C21(H21), C5(H5), C34(H34),
 C36(H36), C48(H48), C15(H15), C3(H3), C9(H9), C4(H4A), C8(H8)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              19086
_shelx_hkl_checksum              75368
_olex2_submission_special_instructions 'No special instructions were received'