Synthesis and properties of cobalt(III) complexes of tripodal ligands containing amide functional groups
Angus, Patricia M.; Elliott, Anthony J.; Sargeson, Alan M.; Willis, Anthony C.; Journal of the Chemical Society, Dalton Transactions  (1999) 1131–; doi:10.1039/a809316d

data_7027198
_publ_section_title
;
 Synthesis and properties of cobalt(III) complexes of tripodal ligands
 containing amide functional groups
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1131
_journal_paper_doi               10.1039/a809316d
_journal_year                    1999
_chemical_formula_moiety         'C11 H21 Co N6, 3(H2 O)'
_chemical_formula_sum            'C11 H27 Co N6 O6'
_chemical_formula_weight         398.30
_chemical_name_systematic
;
[(1,1,1-tris(4-amino-1-oxo-2-azabutyl)ethane)cobalt(III)] trihydrate
;
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      170
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_audit_creation_date             1998-11-17
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
94-02-28  structure finished and report compiled
98-11-18  cif generated from archived files
98-11-18  acw modifies cif
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.040(3)
_cell_length_b                   8.040
_cell_length_c                   43.730(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      49.2
_cell_measurement_theta_min      46.9
_cell_volume                     2448.1(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.12944
_diffrn_orient_matrix_UB_12      -0.02667
_diffrn_orient_matrix_UB_13      0.00702
_diffrn_orient_matrix_UB_21      -0.05968
_diffrn_orient_matrix_UB_22      -0.13074
_diffrn_orient_matrix_UB_23      -0.00941
_diffrn_orient_matrix_UB_31      0.01769
_diffrn_orient_matrix_UB_32      -0.05314
_diffrn_orient_matrix_UB_33      0.01962
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.04984
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3956
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        -1.72
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.650
_exptl_absorpt_correction_T_max  0.338
_exptl_absorpt_correction_T_min  0.244
_exptl_absorpt_correction_type
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1260.00
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details
;
Refinement in space group P 6~1~ with inverted coordinates yielded a higher
R-factor.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.720
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     216
_refine_ls_number_reflns         1090
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/esd_max         0.0060
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0290
_reflns_number_gt                1090
_reflns_number_total             1259
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            809316dsup1.cif
_cod_data_source_block           aje2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00001|Fo|^2^]' 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) + 0.00001|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2447.8(5)
_cod_original_sg_symbol_H-M      'P 65       '
_cod_original_formula_sum        'C11 H27 Co N6 O6 '
_cod_database_code               7027198