Vibrational Spectroscopy and Analysis of Pseudo-tetrahedral Complexes with Metal Imido Bonds
Mehn, Mark P.; Brown, Steven D.; Jenkins, David M.; Peters, Jonas C.; Que, Lawrence; Inorganic Chemistry 45 (2006) 7417–7427; doi:10.1021/ic060670r

data_4332677
_publ_section_title
;
 Vibrational Spectroscopy and Analysis of Pseudo-tetrahedral Complexes
 with Metal Imido Bonds
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7417
_journal_page_last               7427
_journal_paper_doi               10.1021/ic060670r
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C49 H50 B Fe N P3'
_chemical_formula_weight         812.47
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.9378(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7124(13)
_cell_length_b                   19.0114(17)
_cell_length_c                   15.0887(13)
_cell_measurement_temperature    98
_cell_volume                     4189.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21848
_diffrn_reflns_theta_full        28.84
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.614
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         21954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.614
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0886
_reflns_number_gt                16756
_reflns_number_total             21954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060670rsup1.cif
_cod_data_source_block           sdb21twin
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4332677