Structural characterization of the mu-Nitrido Complex {[Fe(OEP)]2N}
Ming Li; W. Robert Scheidt; Journal of Porphyrins and Phthalocyanines 18 (2014) 380–384; doi:10.1142/S1088424614500096

data_1548526
_publ_section_title
;
 Structural characterization of the mu-Nitrido Complex {[Fe(OEP)]2N}
;
_journal_name_full               'Journal of Porphyrins and Phthalocyanines'
_journal_page_first              380
_journal_page_last               384
_journal_paper_doi               10.1142/S1088424614500096
_journal_volume                  18
_journal_year                    2014
_chemical_formula_sum            'C78 H102 Fe2 N9'
_chemical_formula_weight         1277.39
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.614(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9256(19)
_cell_length_b                   13.8434(14)
_cell_length_c                   35.200(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      2.38
_cell_volume                     6740.6(12)
_computing_cell_refinement       madnes
_computing_data_collection       madnes
_computing_data_reduction        'madnes (messerschmitt & pflugraph, 1987)'
_computing_molecular_graphics    'ortep III (burnett, johnson, 1996)'
_computing_publication_material  shelxl-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'enraf-nonius fast area-detector'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            27047
_diffrn_reflns_theta_full        24.28
_diffrn_reflns_theta_max         24.28
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        'no measurable crystal decay'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.9717
_exptl_absorpt_correction_T_min  0.8690
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   DIFABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         10015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+11.3252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                7461
_reflns_number_total             10015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            NIHMS603875-supplement-cif.cif
_cod_data_source_block           sdfeoep2n1
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1548526