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_4334492
_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         'C32 H37 Cl N3 P2 Ru, Cl, 1.5(H2 O)'
_chemical_formula_sum            'C32 H40 Cl2 N3 O1.5 P2 Ru'
_chemical_formula_weight         724.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-20
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_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_b                   9.90919(14)
_cell_length_c                   20.2316(5)
_cell_measurement_reflns_used    8530
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      32.0394
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Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
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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.
;
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olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
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;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9934
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details
;
  1 omega -102.00  -72.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0110  178.0000    0.0000 30

  2 omega  -94.00   -4.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0110  -57.0000  -30.0000 90

  3 omega  -95.00   16.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0110  -19.0000    0.0000 111
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0424062000
_diffrn_orient_matrix_UB_12      -0.0028564000
_diffrn_orient_matrix_UB_13      0.0274454000
_diffrn_orient_matrix_UB_21      0.0169575000
_diffrn_orient_matrix_UB_22      0.0165045000
_diffrn_orient_matrix_UB_23      -0.0258087000
_diffrn_orient_matrix_UB_31      -0.0022832000
_diffrn_orient_matrix_UB_32      0.0695496000
_diffrn_orient_matrix_UB_33      0.0072670000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17028
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         32.11
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70905
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
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empirical absorption correction using spherical harmonics,
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;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.2954
_exptl_crystal_size_mid          0.2458
_exptl_crystal_size_min          0.0541
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9680
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0252P)^2^+1.8078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                8351
_reflns_number_total             9680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302819j_si_002_09.cif
_cod_data_source_block           Complex3e
_cod_original_cell_volume        3108.72(13)
_cod_original_formula_sum        'C32 H40 Cl2 N3 O1.50 P2 Ru'
_cod_database_code               4334492
_chemical_oxdiff_formula         'C32 H37 N3 P2 Cl2 Ru1'
_chemical_oxdiff_usercomment     'Aimee's ajg328-2'
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01