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_4325382
_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_moiety         'C12 H37 Cl Fe n2 P4, (N2H4)0.75'
_chemical_formula_sum            'C12 H40 Cl Fe P4 n3.5'
_chemical_formula_weight         448.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 115.2990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0906(8)
_cell_length_b                   27.982(2)
_cell_length_c                   9.9025(8)
_cell_measurement_reflns_used    5722
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3069
_cell_measurement_theta_min      2.3885
_cell_volume                     2277.3(3)
_computing_cell_refinement       'SAINT Ver. 6.45A  (Bruker-AXS, 2005)'
_computing_data_collection       'SMART Ver. 5.054 (Bruker-AXS, 1998)'
_computing_data_reduction        'SAINT Ver. 6.45A'
_computing_molecular_graphics
;
X-Seed (Barbour, 2001), SHELXTL Ver. 6.14 (Bruker-AXS, 2003)
;
_computing_publication_material  'modiCIFer-12162005 (Guzei, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment
;
attached with Exxon Paratone n, to a short length 
of fibre supported on a thin piece of copper wire 
inserted in a copper mounting pin.  The crystal was 
quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker CCD-1000 area detector'
_diffrn_measurement_method       \w
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22420
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0.10
_diffrn_standards_number         217
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Ver. 2004/1 (Bruker-AXS, 2004)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       needle
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The volume occupied by solvent is  4.9 percent of the unit cell.
;
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         5488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.4214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                4882
_reflns_number_total             5488
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic102519f_si_001.cif
_cod_data_source_block           ldf6pj20
_cod_original_sg_symbol_Hall     '-P 2yn      '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C12 H40 Cl Fe n3.50 P4'
_cod_database_code               4325382