Singlet diradical complexes of chromium, molybdenum, and tungsten with azo anion radical ligands from M(CO)6 precursors.
Sanyal, Anasuya; Chatterjee, Sudipta; Castiñeiras, Alfonso; Sarkar, Biprajit; Singh, Priti; Fiedler, Jan; Zális, Stanislav; Kaim, Wolfgang; Goswami, Sreebrata; Inorganic chemistry 46 (2007) 8584–8593; doi:10.1021/ic700584x

data_4339538
_publ_section_title
;
 Singlet diradical complexes of chromium, molybdenum, and tungsten with
 azo anion radical ligands from M(CO)6 precursors.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8584
_journal_page_last               8593
_journal_paper_doi               10.1021/ic700584x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C56 H44 Mo2 N14 O'
_chemical_formula_weight         1120.93
_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                 93.941(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.887(14)
_cell_length_b                   13.048(14)
_cell_length_c                   30.18(3)
_cell_measurement_reflns_used    908
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.495
_cell_measurement_theta_min      2.29
_cell_volume                     5063(9)
_computing_cell_refinement       'SAINT Software (Bruker, 1997)'
_computing_data_collection       'SMART Software (Bruker, 1997)'
_computing_data_reduction        'SAINT Software (Bruker, 1997)'
_computing_molecular_graphics    'PLATON Spek, 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART CCD-1000'
_diffrn_measurement_method       '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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            51338
_diffrn_reflns_theta_full        25.26
_diffrn_reflns_theta_max         25.26
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.9318
_exptl_absorpt_correction_T_min  0.8791
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.709
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         8891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0334P)^2^+35.4551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1743
_reflns_number_gt                4760
_reflns_number_total             8891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700584x-file002.cif
_cod_data_source_block           03acsg01
_cod_original_sg_symbol_H-M      'P2(1)/c (No. 14)'
_cod_database_code               4339538