Base-Induced Dehydrogenation of Ruthenium Hydrazine Complexes
Leslie D. Field; Hsiu L. Li; Scott J. Dalgarno; Ruaraidh D. McIntosh; Inorganic Chemistry 52 (2013) 1570–1583; doi:10.1021/ic302449n

data_4333740
_publ_section_title
;
 Base-Induced Dehydrogenation of Ruthenium Hydrazine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1570
_journal_page_last               1583
_journal_paper_doi               10.1021/ic302449n
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C43 H48 Cl N2 P4 Ru), C4 H8 O, 2(Cl)'
_chemical_formula_sum            'C90 H104 Cl4 N4 O P8 Ru2'
_chemical_formula_weight         1849.47
_chemical_name_common            LHL2783
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_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            8
_cell_length_a                   17.3284(9)
_cell_length_b                   26.8150(12)
_cell_length_c                   36.139(3)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.53
_cell_volume                     16792.4(18)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            125524
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.8743
_exptl_absorpt_correction_T_min  0.8197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       Block
_exptl_crystal_F_000             7648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9285
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+34.0162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                8177
_reflns_number_total             9285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302449n_si_001_5.cif
_cod_data_source_block           LHL2783
_cod_original_cell_volume        16792.2(16)
_cod_database_code               4333740