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_4323720
_publ_contact_author
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        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
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_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
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 The Chemistry of 1,3,5-Triazacyclohexane Complexes. 6.1Synthesis and
 Characterization of the Cobalt(II) Methoxide Core {Co3(OMe)4}2+
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_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         '[C6 H16 N3]+[Cl]-'
_chemical_formula_structural     '[(CH3)3 (C3 N3 H6)]*[H Cl]'
_chemical_formula_sum            'C6 H16 Cl N3'
_chemical_formula_weight         165.67
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.0366(9)
_cell_length_b                   12.2986(6)
_cell_length_c                   13.9949(7)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.3
_cell_measurement_theta_min      13.5
_cell_volume                     1899.6(2)
_computing_cell_refinement       'STADI4 (STOE, 1995)'
_computing_data_collection       'STADI4 (STOE, 1995)'
_computing_data_reduction        'X-RED, (STOE, 1995)'
_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      293(2)
_diffrn_measurement_device       'STOE Stadi4 Diffractometer'
_diffrn_measurement_method       \w-2\q
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4061
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        3.1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          1.1
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.162
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_restrained_S_obs      1.162
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_obs          0.0463
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1600
_refine_ls_wR_factor_obs         0.1179
_reflns_number_observed          1386
_reflns_number_total             2178
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9704593_1.cif
_cod_data_source_block           rdk17
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0785P)^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^)+(0.0785P)^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 
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_cod_database_code               4323720