The Chemistry of 1,3,5-Triazacyclohexane Complexes. 6.1Synthesis and Characterization of the Cobalt(II) Methoxide Core {Co3(OMe)4}2+
Randolf D. Köhn; Matthias Haufe; Gabriele Kociok-Köhn; Alexander C. Filippou; Inorganic Chemistry 36 (1997) 6064–6069; doi:10.1021/ic9704593

data_4323722
_publ_contact_author
;
        Randolf D. K\"ohn
        Institut f\"ur Anorganische und Analytische Chemie
        Technische Universit\"at Berlin
        Stra\&se des 17. Juni 135
        10623 Berlin
        Bundesrepublik Deutschland
;
_publ_contact_author_email       kociok@wap0203.chem.tu-berlin.de
_publ_contact_author_fax         '049 30 314-22168'
_publ_contact_author_phone       '049 30 314-26203'
_publ_section_title
;
 The Chemistry of 1,3,5-Triazacyclohexane Complexes. 6.1Synthesis and
 Characterization of the Cobalt(II) Methoxide Core {Co3(OMe)4}2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6064
_journal_page_last               6069
_journal_paper_doi               10.1021/ic9704593
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        CH2Cl2
_chemical_formula_moiety         '[C22 H57 Co3 N9 O4][B C24 F20]2*(CH2 Cl2)'
_chemical_formula_structural
;
 [{(CH3)3 (C3 H6 N3) Co}3 (O (CH3))4][B (C6 F5)4]2 *(CH2 Cl2)
;
_chemical_formula_sum            'C71 H59 B2 Cl2 Co3 F40 N9 O4'
_chemical_formula_weight         2131.58
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                79.23(2)
_cell_angle_beta                 76.855(13)
_cell_angle_gamma                70.10(2)
_cell_formula_units_Z            2
_cell_length_a                   13.857(2)
_cell_length_b                   16.843(3)
_cell_length_c                   19.318(2)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     4098.8(12)
_computing_cell_refinement       'IPDS (STOE, 1996)'
_computing_data_collection       'IPDS (STOE, 1996)'
_computing_data_reduction        'IPDS (Software 2.65, 1996)'
_computing_molecular_graphics
;
 L.Zsolnai,H.Pritzkow, ZORTEP, ORTEP program for PC,
 Universit\"at Heidelberg 1994
;
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f-rotation
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28874
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         2.18
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             2130
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.957
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1227
_refine_ls_number_reflns         15024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_obs          0.0348
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0917
_refine_ls_wR_factor_obs         0.0848
_reflns_number_observed          11549
_reflns_number_total             15032
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9704593_3.cif
_cod_data_source_block           rdk23
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4098.9(10)
_cod_database_code               4323722