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_4334493
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H39 Cl N3 P2 Ru, 3(C H4 O), Cl'
_chemical_formula_sum            'C39 H51 Cl2 N3 O3 P2 Ru'
_chemical_formula_weight         843.74
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-08-02
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.141(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3263(7)
_cell_length_b                   8.5294(2)
_cell_length_c                   26.4162(13)
_cell_measurement_reflns_used    13940
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      30.0000
_cell_measurement_theta_min      2.8920
_cell_volume                     3900.9(3)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_details
;
  1 omega  -46.00   52.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9870   37.0000 -180.0000 98

  2 omega  -38.00    7.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9870  -77.0000   30.0000 45

  3 omega  -90.00  -63.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9870  -77.0000   30.0000 27

  4 omega  -47.00  -21.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2370  -72.0000  120.0000 26

  5 omega   -8.00   43.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2370   81.0000   -8.0000 51

  6 omega   16.00   50.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2375   72.0000   59.0000 34

  7 omega   52.00   82.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2375   77.0000 -120.0000 30

  8 omega  -44.00    7.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9875  -72.0000  109.0000 51

  9 omega  -80.00  -39.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9875  137.0000 -104.0000 41

 10 omega   14.00   41.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2375  -72.0000  120.0000 27

 11 omega   22.00   48.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2375  -81.0000   49.0000 26

 12 omega  -32.00   68.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2375    0.0000 -120.0000 100
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0159265000
_diffrn_orient_matrix_UB_12      -0.0667471000
_diffrn_orient_matrix_UB_13      0.0085957000
_diffrn_orient_matrix_UB_21      0.0335101000
_diffrn_orient_matrix_UB_22      -0.0060852000
_diffrn_orient_matrix_UB_23      0.0229918000
_diffrn_orient_matrix_UB_31      -0.0174813000
_diffrn_orient_matrix_UB_32      0.0493987000
_diffrn_orient_matrix_UB_33      0.0144003000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22702
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.981
_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_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_recrystallization_method 'MeOH slow evaporation'
_exptl_crystal_size_max          0.1549
_exptl_crystal_size_mid          0.1457
_exptl_crystal_size_min          0.0797
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         9763
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.2732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                9397
_reflns_number_total             9763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302819j_si_002_10.cif
_cod_data_source_block           Complex3f
_cod_database_code               4334493
_chemical_oxdiff_formula         C36H39Cl2N3P2Ru
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50