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_4330427
_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            'C55.5 H60 B Fe N2 O2 P3'
_chemical_formula_weight         946.62
_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                68.4530(10)
_cell_angle_beta                 69.9450(10)
_cell_angle_gamma                64.3070(10)
_cell_formula_units_Z            2
_cell_length_a                   12.74930(10)
_cell_length_b                   13.26200(10)
_cell_length_c                   17.4092(2)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.03
_cell_measurement_theta_min      2.80
_cell_volume                     2407.19(5)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 3.0 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26019
_diffrn_reflns_theta_full        63.68
_diffrn_reflns_theta_max         63.68
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    3.794
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.3586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         7698
_refine_ls_number_restraints     1297
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0502P)^2^+1.3178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                6534
_reflns_number_total             7698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301704f_si_002_05.cif
_cod_data_source_block           8
_cod_original_cell_volume        2407.19(4)
_cod_original_formula_sum        'C55.50 H60 B Fe N2 O2 P3'
_cod_database_code               4330427