cis-1,3,5-Triaminocyclohexane as a Facially Capping Ligand for Ruthenium(II)
Aimee J. Gamble; Jason M. Lynam; Robert J. Thatcher; Paul H. Walton; Adrian C. Whitwood; Inorganic Chemistry 52 (2013) 4517–4527; doi:10.1021/ic302819j

data_4334490
_publ_contact_author_address
;Department of Chemistry
University of York
Heslington 
York
YO10 5DD
UK
;
_publ_contact_author_email       jason.lynam@york.ac.uk
_publ_contact_author_fax         +44(0)1904322516
_publ_contact_author_name        'Jason Lynam'
_publ_contact_author_phone       +44(0)1904322534
_publ_section_title
;
 cis-1,3,5-Triaminocyclohexane as a Facially Capping Ligand for
 Ruthenium(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4517
_journal_page_last               4527
_journal_paper_doi               10.1021/ic302819j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C33 H41 Cl N3 P2 Ru, C H4 O, 1.87(H2 O), Cl, 0.13(O)'
_chemical_formula_sum            'C34 H48.75 Cl2 N3 O3 P2 Ru'
_chemical_formula_weight         781.42
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-10
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.431(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.70362(19)
_cell_length_b                   20.1181(4)
_cell_length_c                   17.9253(4)
_cell_measurement_reflns_used    9494
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      32.0785
_cell_measurement_theta_min      2.9154
_cell_volume                     3488.89(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details
;
  1 omega  -41.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2610  -77.0000   60.0000 93

  2 omega    0.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2610  -37.0000  -60.0000 39

  3 omega    3.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2610   77.0000 -180.0000 89
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0444546000
_diffrn_orient_matrix_UB_12      0.0242529000
_diffrn_orient_matrix_UB_13      0.0140473000
_diffrn_orient_matrix_UB_21      0.0336701000
_diffrn_orient_matrix_UB_22      -0.0039292000
_diffrn_orient_matrix_UB_23      0.0362594000
_diffrn_orient_matrix_UB_31      0.0476739000
_diffrn_orient_matrix_UB_32      0.0252851000
_diffrn_orient_matrix_UB_33      -0.0078065000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18989
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.15
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            '? yellow'
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             1623
_exptl_crystal_recrystallization_method MeOH
_exptl_crystal_size_max          0.1919
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.1156
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         10808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+1.7636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                9123
_reflns_number_total             10808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302819j_si_002_07.cif
_cod_data_source_block           Complex3c
_cod_database_code               4334490
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01