Synthesis, structure and redox properties of a new ruthenium(II) complex containing the flexible tridentate ligand N,N-bis(2-pyridylmethyl)ethylamine, cis-fac-Ru(bpea)22+, and its homologue attached covalently to a polypyrrole film
Isabel Romero; Montserrat Rodríguez; Antoni Llobet; Marie-Noëlle Collomb-Dunand-Sauthier; Alain Deronzier; Teodor Parella; Helen Stoeckli-Evans; J. Chem. Soc., Dalton Trans.  (2000) 1689–1694; doi:10.1039/a909511j

data_7009230
_publ_section_title
;
 Synthesis, structure and redox properties of a new ruthenium(II)
 complex containing the flexible tridentate ligand
 N,N-bis(2-pyridylmethyl)ethylamine, cis-fac-Ru(bpea)22+, and its
 homologue attached covalently to a polypyrrole film
;
_journal_issue                   11
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1689
_journal_page_last               1694
_journal_paper_doi               10.1039/a909511j
_journal_year                    2000
_chemical_formula_sum            'C31 H38.5 F12 N7.5 P2 Ru'
_chemical_formula_weight         907.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-A 2yab'
_symmetry_space_group_name_H-M   'A 1 2/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                 97.861(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.4749(13)
_cell_length_b                   11.6232(6)
_cell_length_c                   41.920(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      1.96
_cell_volume                     7469.2(10)
_computing_cell_refinement       'CELL (Stoe & Cie GmbH, Darmstadt,1997)'
_computing_data_collection       'EXPOSE (Stoe & Cie GmbH, Darmstadt,1997)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie GmbH,Darmstadt, 1997)'
_computing_molecular_graphics    'PLATON/PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.473
_diffrn_measured_fraction_theta_max 0.473
_diffrn_measurement_device_type  'STOE Image Plate Diffraction System'
_diffrn_measurement_method       'phi rotation scans'
_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  0.0971
_diffrn_reflns_av_sigmaI/netI    0.1434
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            28119
_diffrn_reflns_theta_full        25.89
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.000044(16)
_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   0.757
_refine_ls_hydrogen_treatment    'riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.757
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                3735
_reflns_number_total             7224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909511j.txt
_cod_data_source_block           cpd1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0333P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7469.3(10)
_cod_original_sg_symbol_H-M      'A 2/n'
_cod_original_formula_sum        'C31 H38.50 F12 N7.50 P2 Ru'
_cod_database_code               7009230