Tautomerization of Methyldiazene to Formaldehyde-Hydrazone in Ruthenium and Osmium Complexes
Gabriele Albertin; Stefano Antoniutti; Alessia Bacchi; Fabiola De Marchi; Giancarlo Pelizzi; Inorganic Chemistry 44 (2005) 8947–8954; doi:10.1021/ic050817z

data_4310050
_publ_section_title
;
Tautomerization of Methyldiazene to Formaldehyde-Hydrazone in Ruthenium and
Osmium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8947
_journal_page_last               8954
_journal_paper_doi               10.1021/ic050817z
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C74.5 H105 B2 Cl N2 O13 P4 Ru'
_chemical_formula_weight         1518.62
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2390(10)
_cell_length_b                   19.0410(10)
_cell_length_c                   19.5380(10)
_cell_measurement_temperature    293(2)
_cell_volume                     8273.4(7)
_computing_cell_refinement
;
SAINT: SAX, Area Detector Integration, Siemens Analytical instruments
INC., Madison, Wisconsin, USA. 
;
_computing_data_collection
;
SAINT: SAX, Area Detector Integration, Siemens Analytical instruments
 INC., Madison, Wisconsin, USA. 
;
_computing_data_reduction
;
SAINT: SAX, Area Detector Integration, Siemens Analytical instruments
 INC., Madison, Wisconsin, USA. 
SADABS: Siemens Area Detector Absorption Correction Software, 
Sheldrick G., 1996, University of Goettingen, Germany.
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'PARST -  M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
Burla M.C., Camalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., 
Polidori, G. & Spagna, R. (2001). J. Appl. Cryst. - 34, 523-526. 
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS CCD diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56361
_diffrn_reflns_theta_full        21.57
_diffrn_reflns_theta_max         21.57
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.882367
_exptl_absorpt_correction_type   'symmetry-related measurements'
_exptl_absorpt_process_details
'according to procedures implemented in the SADABS package'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3204
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.072
_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   0.957
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         9553
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.148
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                6881
_reflns_number_total             9553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050817zsi20050520_083155.cif
_cod_data_source_block           compound-5
_cod_original_formula_sum        'C74.50 H105 B2 Cl N2 O13 P4 Ru'
_cod_database_code               4310050