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_7004228
_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            'C50.5 H56 B Cl5 F4 N4 P2 Ru'
_chemical_formula_weight         1146.06
_chemical_name_common            'in paper 2'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.428(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3337(4)
_cell_length_b                   17.2454(5)
_cell_length_c                   21.8269(7)
_cell_measurement_temperature    150(2)
_cell_volume                     5247.9(3)
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28511
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.8403
_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    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.822
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0121(9)
_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   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         9076
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+23.7411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.1875
_reflns_number_gt                7505
_reflns_number_total             9076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804572k.txt
_cod_data_source_block           c:\x-rays~1\finish~1\andrew~1\alg3\alg3
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C50.50 H56 B Cl5 F4 N4 P2 Ru'
_cod_database_code               7004228