Controlling the binding of dihydrogen using ruthenium complexes containing N-mono-functionalised 1,4,7-triazacyclononane ligand systems
Gott, Andrew L.; McGowan, Patrick C.; Podesta, Thomas J.; Dalton Transactions  (2008) 3729–3738; doi:10.1039/b804572k

data_7004229
_publ_section_title
;
 Controlling the binding of dihydrogen using ruthenium complexes
 containing N-mono-functionalised 1,4,7-triazacyclononane ligand
 systems
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              3729
_journal_page_last               3738
_journal_paper_doi               10.1039/b804572k
_journal_year                    2008
_chemical_formula_sum            'C92 H110 B2 Cl0 F8 N6 O4 P4 Ru2'
_chemical_formula_weight         1863.50
_chemical_name_common            'in paper 4'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.74
_cell_angle_beta                 111.43
_cell_angle_gamma                108.2990(10)
_cell_formula_units_Z            2
_cell_length_a                   14.88850(10)
_cell_length_b                   18.62980(10)
_cell_length_c                   19.9116(2)
_cell_measurement_temperature    150(2)
_cell_volume                     4814.86(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
'Nonius KappaCCD area detector diffractometer'
;
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            100011
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_correction_T_min  0.8490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.912
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.0014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1122
_refine_ls_number_reflns         21956
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+9.1024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1950
_reflns_number_gt                17437
_reflns_number_total             21956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804572k.txt
_cod_data_source_block           c:\x-rays~1\finish~1\andrew~1\alg12\alg12
_cod_original_cell_volume        4814.85(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004229