Dinitrosyl Iron Complexes Relevant to Rieske Cluster Nitrosylation
Zachary J. Tonzetich; Loi H. Do; Stephen J. Lippard; Journal of the American Chemical Society 131 (2009) 7964–7965; doi:10.1021/ja9030159

data_4104543
_publ_section_title
;
 Dinitrosyl Iron Complexes Relevant to Rieske Cluster Nitrosylation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7964
_journal_page_last               7965
_journal_paper_doi               10.1021/ja9030159
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C65 H71 Fe N5 O2 P2'
_chemical_formula_weight         1072.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.406(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7691(11)
_cell_length_b                   19.300(2)
_cell_length_c                   27.719(3)
_cell_measurement_reflns_used    4233
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.27
_cell_volume                     5759.5(10)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13535
_diffrn_reflns_theta_full        26.68
_diffrn_reflns_theta_max         26.68
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9609
_exptl_absorpt_correction_T_min  0.8951
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0011(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         13535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1344P)^2^+5.5735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2063
_reflns_number_gt                11487
_reflns_number_total             13535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9030159_si_002_2.cif
_cod_data_source_block           PPNDNIC
_cod_original_cell_volume        5759.7(10)
_cod_database_code               4104543