Triphos derivatives and diphosphines as ligands in the ruthenium-catalysed alcohol amination with NH3.
Nakagawa, N.; Derrah, E. J.; Schelwies, M.; Rominger, F.; Trapp, O.; Schaub, T.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6856–6865; doi:10.1039/c5dt04870b

data_7038373
_publ_section_title
;
 Triphos derivatives and diphosphines as ligands in the
 ruthenium-catalysed alcohol amination with NH3.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6856
_journal_page_last               6865
_journal_paper_doi               10.1039/c5dt04870b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C49 H48 Cl3 O2 P3 Ru'
_chemical_formula_weight         969.20
_chemical_name_common            'E in manuscript'
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-03 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4486(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8254(8)
_cell_length_b                   26.2437(18)
_cell_length_c                   14.7497(10)
_cell_measurement_reflns_used    8323
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.27
_cell_volume                     4563.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51234
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.239
_diffrn_reflns_theta_min         1.552
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.8323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.852
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         12377
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+5.2848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8429
_reflns_number_total             12377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04870b2.cif
_cod_data_source_block           nn1
_cod_depositor_comments
'Adding full bibliography for 7038370--7038373.cif.'
_cod_database_code               7038373
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              38178