Synthesis and Characterization of Iron(II) and Ruthenium(II) Hydrido Hydrazine Complexes
Leslie D. Field; Hsiu L. Li; Scott J. Dalgarno; Paul Jensen; Ruaraidh D. McIntosh; Inorganic Chemistry 50 (2011) 5468–5476; doi:10.1021/ic102519f

data_4325384
_publ_section_title
;
 Synthesis and Characterization of Iron(II) and Ruthenium(II) Hydrido
 Hydrazine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5468
_journal_page_last               5476
_journal_paper_doi               10.1021/ic102519f
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C36 H57 B P4 Ru n2'
_chemical_formula_weight         753.60
_chemical_name_common            X83339
_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   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.759(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.252(3)
_cell_length_b                   18.373(4)
_cell_length_c                   15.893(4)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.13
_cell_measurement_theta_min      2.57
_cell_volume                     3824.5(15)
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker nonius 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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            70455
_diffrn_reflns_theta_full        36.57
_diffrn_reflns_theta_max         36.57
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.8887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       Block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.663
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         18153
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0307P)^2^+0.1457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                12547
_reflns_number_total             18153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102519f_si_003.cif
_cod_data_source_block           X83339
_cod_original_cell_volume        3824.5(14)
_cod_original_formula_sum        'C36 H57 B n2 P4 Ru'
_cod_database_code               4325384