Synthesis, crystal structure and catalytic activity in reductive amination of dichlorido(η^6^-<i>p</i>-cymene)(2'-dicyclohexylphosphanyl-2,6-dimethoxybiphenyl-κ<i>P</i>)ruthenium(II)
Makarova, Maria; Tsygankov, Alexey A.; Chusova, Olga; Linko, Ivan V.; Dorovatovskii, Pavel V.; Zubavichus, Yan V.; Acta Crystallographica Section E 74 (2018) 487–491; doi:10.1107/S2056989018003821

data_2242416
_publ_section_title
;
 Synthesis, crystal structure and catalytic activity in reductive
 amination of
 dichlorido(\h^6^-<i>p</i>-cymene)(2'-dicyclohexylphosphanyl-2,6-dimethoxybiphenyl-\k<i>P</i>)ruthenium(II)
;
_journal_coeditor_code           SU5428
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              487
_journal_page_last               491
_journal_paper_doi               10.1107/S2056989018003821
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Ru Cl2 (C10 H14) (C26 H35 O2 P)]'
_chemical_formula_moiety         'C36 H49 Cl2 O2 P Ru'
_chemical_formula_sum            'C36 H49 Cl2 O2 P Ru'
_chemical_formula_weight         716.69
_chemical_name_systematic
Dichlorido(\h^6^-<i>p</i>-cymene)(2'-dicyclohexylphosphanyl-2,6-dimethoxybiphenyl-\k<i>P</i>)ruthenium(II)
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 118.17(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.790(4)
_cell_length_b                   19.950(4)
_cell_length_c                   20.225(4)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      3.2
_cell_volume                     7039(3)
_computing_cell_refinement
;
<i>iMosflm</i> (Battye <i>et al.</i>,  2011)
;
_computing_data_collection
;
<i>MARCCD</i> (Doyle, 2011)
;
_computing_data_reduction
;
<i>iMosflm</i> (Battye <i>et al.</i>,  2011)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL (Sheldrick, 2015b), PLATON (Spek, 2009) and
publCIF(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96260
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            85347
_diffrn_reflns_theta_full        35.279
_diffrn_reflns_theta_max         38.443
_diffrn_reflns_theta_min         3.199
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SCALA; Evans, 2006)
;
_exptl_crystal_colour            dark-orange
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prism
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.773
_refine_ls_extinction_coef       0.00120(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         15331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0738P)^2^+8.8P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                11898
_reflns_number_total             15331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5428sup1.cif
_cod_data_source_block           I
_cod_database_code               2242416
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.855
_shelx_hkl_checksum              23557
_shelx_res_checksum              47127
_shelxl_version_number           2014/6
_cod_database_fobs_code 2242416