Synthesis and Characterization of a Chromium(V) cis-Dioxo Bis(1,10-phenanthroline) Complex and Crystal and Molecular Structures of Its Chromium(III) Precursor
Colin L. Weeks; Aviva Levina; Carolyn T. Dillon; Peter Turner; Ronald R. Fenton; Peter A. Lay; Inorganic Chemistry 43 (2004) 7844–7856; doi:10.1021/ic049008q

data_4312072
_publ_contact_author_address
;    
 Centre for Heavy Metals Research
 School of Chemistry
 The University of Sydney
 NSW 2006
 Australia
;
_publ_contact_author_email       p.lay@chem.usyd.edu.au
_publ_contact_author_fax         '61 2 9351 3329'
_publ_contact_author_name        'Peter A. Lay'
_publ_contact_author_phone       '61 2 9351 4269'
_publ_section_title
;
 Synthesis and Characterization of a Chromium(V) cis-Dioxo
 Bis(1,10-phenanthroline) Complex and Crystal and Molecular Structures of
 Its Chromium(III) Precursor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7844
_journal_page_last               7856
_journal_paper_doi               10.1021/ic049008q
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C24 H20 Cr N4 O2, 3(N O3), 2(H2 O), O0.5'
_chemical_formula_sum            'C24 H24 Cr N7 O13.5'
_chemical_formula_weight         678.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5923(5)
_cell_length_b                   32.8173(16)
_cell_length_c                   9.0928(5)
_cell_measurement_reflns_used    4587
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.884
_cell_measurement_theta_min      2.212
_cell_volume                     2862.4(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        'SAINT and XPREP'
_computing_molecular_graphics    'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26316
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         75
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6669
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.1742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                5788
_reflns_number_total             6669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049008qsi20040722_064819.cif
_cod_data_source_block           pal39
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C24 H24 Cr N7 O13.50'
_cod_database_code               4312072