Dinuclear Triple Helicates with Diazine Ligands: X-ray Structural, Electrochemical, and Magnetic Studies
Subramanya Gupta Sreerama; Samudranil Pal; Inorganic Chemistry 44 (2005) 6299–6307; doi:10.1021/ic050704f

data_4309532
_publ_section_title
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Dinuclear Triple Helicates with Diazine Ligands: X-ray Structural,
Electrochemical, and Magnetic Studies
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6299
_journal_page_last               6307
_journal_paper_doi               10.1021/ic050704f
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C48 H46 Co2 N8 O9'
_chemical_formula_weight         996.79
_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                62.8450(10)
_cell_angle_beta                 66.8460(10)
_cell_angle_gamma                65.9400(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5167(8)
_cell_length_b                   14.8098(9)
_cell_length_c                   15.1124(9)
_cell_measurement_reflns_used    6231
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.61
_cell_volume                     2200.8(2)
_computing_cell_refinement       'Bruker SMART (2003)'
_computing_data_collection       'Bruker SMART (2003) '
_computing_data_reduction        'Bruker SAINT-Plus (2003)'
_computing_molecular_graphics    'ORTEX6a (McArdle,1995), PLATON (Spek,2002)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.730
_diffrn_measured_fraction_theta_max 0.730
_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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.1216
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18608
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.9223
_exptl_absorpt_correction_T_min  0.7291
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                4560
_reflns_number_total             7991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050704fsi20050505_023049_1.cif
_cod_data_source_block           '[Co2(salhn)3].2(CH3)2NCHO.H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4309532