Synthesis and structure of mono-, bi- and trimetallic amine-bis(phenolate) cobalt(II) complexes.
Das, Uttam K.; Bobak, Julia; Fowler, Candace; Hann, Sarah E.; Petten, Chad F.; Dawe, Louise N.; Decken, Andreas; Kerton, Francesca M.; Kozak, Christopher M.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 5462–5477; doi:10.1039/c002843f

data_7025696
_publ_section_title
;
 Synthesis and structure of mono-, bi- and trimetallic
 amine-bis(phenolate) cobalt(II) complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5462
_journal_page_last               5477
_journal_paper_doi               10.1039/c002843f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety
'2(C40 H58 N2 O2), 2Co, 2(C H3 O H), 3(C7 H8)'
_chemical_formula_sum            'C103 H148 Co2 N4 O6'
_chemical_formula_weight         1656.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                100.085(3)
_cell_angle_beta                 97.893(3)
_cell_angle_gamma                105.592(4)
_cell_formula_units_Z            1
_cell_length_a                   10.346(3)
_cell_length_b                   15.283(5)
_cell_length_c                   15.482(5)
_cell_measurement_reflns_used    7090
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.6346
_cell_measurement_theta_min      1.7348
_cell_volume                     2277.2(12)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.1187
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17963
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.9387
_exptl_absorpt_correction_T_min  0.8507
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 154 electrons per
unit cell in one void (total volume 624 ^A^3); that is 154 electrons
per formula unit (with Z=1 in this model). Disordered solvent lattice
toluene molecules were present prior to the application of Squeeze,
however, a satisfactory point atom model could not be achieved.
The application of Squeeze gave a good improvement in the data
statistics and allowed for a full anisotropic refinement of the
structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         9168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0562
_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^)+(0.1222P)^2^+0.9085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1794
_reflns_number_gt                8618
_reflns_number_total             9168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002843f.txt
_cod_data_source_block           3CH3OH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2277.1(13)
_cod_database_code               7025696