Radical Anions of Metallo-organic Diazines: Structural, Spectroscopic, and Theoretical Investigation of a Pyrazyl Radical Anion
Choua, Sylvie; Djukic, Jean-Pierre; Dalléry, Jérôme; Welter, Richard; Turek, Philippe; Ricard, Louis; Organometallics 28 (2009) 6194–; doi:10.1021/om900668n

data_4070231
_publ_section_title
;
 Radical Anions of Metallo-organic Diazines: Structural, Spectroscopic,
 and Theoretical Investigation of a Pyrazyl Radical Anion
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6194
_journal_paper_doi               10.1021/om900668n
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety
'C44 H38 Mn2 N2 O6, 2(C18 H36 K N2 O6), C5 Mn O5'
_chemical_formula_sum            'C85 H110 K2 Mn3 N6 O23'
_chemical_formula_weight         1826.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 92.456(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.050(1)
_cell_length_b                   12.672(1)
_cell_length_c                   19.071(1)
_cell_measurement_reflns_used    8812
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     4358.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22423
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_correction_T_min  0.8793
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1918
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6917
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                4408
_reflns_number_total             6917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900668n_si_002.cif
_cod_data_source_block           '[(222)K]2[Mn(CO)5][2b]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P2/n     '
_cod_database_code               4070231