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_4334489
_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         'C32 H39 Cl N3 P2 Ru, F6 P'
_chemical_formula_sum            'C32 H39 Cl F6 N3 P3 Ru'
_chemical_formula_weight         809.09
_space_group_crystal_system      trigonal
_space_group_IT_number           158
_space_group_name_Hall           'P 3 -2"c'
_space_group_name_H-M_alt        'P 3 c 1'
_symmetry_space_group_name_Hall  'P 3 -2"c'
_symmetry_space_group_name_H-M   'P 3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-04-27
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_cell_length_b                   18.9550(7)
_cell_length_c                   16.9765(6)
_cell_measurement_reflns_used    5537
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      29.0017
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
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(compiled Oct 25 2010,18:11:34)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
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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.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'smtbx-flip (Bourhis, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_details
;
  1 omega  -50.00  -11.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6140  133.0000  -64.0000 39

  2 omega  -50.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8640  -37.0000  150.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_12      0.0376736000
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_diffrn_orient_matrix_UB_21      -0.0383702000
_diffrn_orient_matrix_UB_22      -0.0020945000
_diffrn_orient_matrix_UB_23      -0.0025970000
_diffrn_orient_matrix_UB_31      0.0076437000
_diffrn_orient_matrix_UB_32      0.0209681000
_diffrn_orient_matrix_UB_33      0.0363921000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
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_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11946
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         3.22
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92544
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       needle
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.1754
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.0707
_platon_squeeze_details
;
;
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         5256
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0518P)^2^+3.2160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                4643
_reflns_number_total             5256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302819j_si_002_06.cif
_cod_data_source_block           Complex3b
_cod_original_cell_volume        5282.3(5)
_cod_database_code               4334489
_chemical_oxdiff_formula         'C33 H41 Cl F6 N3 P3 Ru'
_chemical_oxdiff_usercomment     'Aimee's ajg263'
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32