Atom Transfer as a Preparative Tool in Coordination Chemistry. Synthesis and Characterization of Cr(V) Nitrido Complexes of Bidentate Ligands
Torben Birk; Jesper Bendix; Inorganic Chemistry 42 (2003) 7608–7615; doi:10.1021/ic034777f

data_4312505
_publ_contact_author
; 
Jesper Bendix
University of Copenhagen
Department of Chemistry 
Universitetsparken 5
DK-2100
Denmark 
;
_publ_contact_author_email       Bendix@kiku.dk
_publ_contact_author_fax         '45 35320133'
_publ_contact_author_phone       '45 35320101'
_publ_section_title
;
 Atom Transfer as a Preparative Tool in Coordination Chemistry. Synthesis
 and Characterization of Cr(V) Nitrido Complexes of Bidentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7608
_journal_page_last               7615
_journal_paper_doi               10.1021/ic034777f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C30 H22 Cr N O4'
_chemical_formula_sum            'C30 H22 Cr N O4'
_chemical_formula_weight         512.49
_chemical_name_systematic
; 
bis(dibenzoylmethanoato)nitrido-chromium(V) 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and manual editing'
_cell_angle_alpha                90.000(11)
_cell_angle_beta                 90.000(7)
_cell_angle_gamma                90.000(6)
_cell_formula_units_Z            8
_cell_length_a                   14.6940(6)
_cell_length_b                   16.4570(18)
_cell_length_c                   19.890(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4809.8(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            193667
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.223
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0351P)^2^+7.2191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                5608
_reflns_number_total             7007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034777fsi20030707_095115_2.cif
_cod_data_source_block           dbm
_cod_original_cell_volume        4809.8(8)
_cod_database_code               4312505