Mononuclear Five- and Six-Coordinate Iron Hydrazido and Hydrazine Species
Caroline T. Saouma; Connie C. Lu; Jonas C. Peters; Inorganic Chemistry 51 (2012) 10043–10054; doi:10.1021/ic301704f

data_4330423
_publ_section_title
;
 Mononuclear Five- and Six-Coordinate Iron Hydrazido and Hydrazine Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10043
_journal_page_last               10054
_journal_paper_doi               10.1021/ic301704f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C234 H178 B2 Cl1.94 Fe1.94 P6 Tl0.06'
_chemical_formula_weight         3386.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.466(2)
_cell_angle_beta                 80.341(2)
_cell_angle_gamma                77.215(2)
_cell_formula_units_Z            1
_cell_length_a                   13.5781(10)
_cell_length_b                   15.8816(11)
_cell_length_c                   22.2863(16)
_cell_measurement_reflns_used    4705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      2.24
_cell_volume                     4504.5(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19581
_diffrn_reflns_theta_full        13.15
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.747422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             1770
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1173
_refine_ls_number_reflns         12901
_refine_ls_number_restraints     1365
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1538
_refine_ls_R_factor_gt           0.0914
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+12.7100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2460
_reflns_number_gt                7575
_reflns_number_total             12901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301704f_si_002_01.cif
_cod_data_source_block           FeCl
_cod_database_code               4330423