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_4339537
_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_moiety         'C34 H26 N8 W'
_chemical_formula_sum            'C34 H26 N8 W'
_chemical_formula_weight         730.48
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.058(2)
_cell_angle_beta                 104.629(2)
_cell_angle_gamma                89.990(2)
_cell_formula_units_Z            4
_cell_length_a                   10.4134(14)
_cell_length_b                   17.031(2)
_cell_length_c                   16.337(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2803.4(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'Bruker SAINT PLUS'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97(Altomare, et. al. 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18772
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    4.161
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.583
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         13278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                11572
_reflns_number_total             13278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700584x-file003.cif
_cod_data_source_block           22deca
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2803.4(7)
_cod_original_sg_symbol_H-M      P-1(no.2)
_cod_database_code               4339537