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_7004232
_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            'C30 H39 B2 F8 N4 O2 P Ru'
_chemical_formula_weight         793.31
_chemical_name_common            'in paper 9'
_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                90.3360(10)
_cell_angle_beta                 96.8480(11)
_cell_angle_gamma                113.4930(10)
_cell_formula_units_Z            2
_cell_length_a                   9.59150(10)
_cell_length_b                   10.23540(10)
_cell_length_c                   18.2375(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1627.50(4)
_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_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29394
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.9191
_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    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.277
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+1.0155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                5773
_reflns_number_total             6362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804572k.txt
_cod_data_source_block           alg6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004232