An unusual pendant-arm macrocycle formed by condensation of a cobalt(iii) tripodal complex with methanal
Angus, Patricia M.; Geue, Rodney J.; Jensen, Niels K. B.; Larsen, F. Krebs; Jin Qin, Chang; Sargeson, Alan M.; Journal of the Chemical Society, Dalton Transactions  (2002) 4260–; doi:10.1039/b205832d

data_7011918
_publ_section_title
;
 An unusual pendant-arm macrocycle formed by condensation of a
 cobalt(iii) tripodal complex with methanal
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4260
_journal_paper_doi               10.1039/b205832d
_journal_year                    2002
_chemical_compound_source        'Alan M. Sargeson'
_chemical_formula_moiety         'C13 H30 Cl Co N3 O S3, 3(Cl O4), 3(H2 O)'
_chemical_formula_sum            'C13 H36 Cl4 Co N3 O16 S3'
_chemical_formula_weight         787.46
_chemical_name_systematic
;
8-(4'-ammonio-2'-thiabutyl)-8-methyl-1-oxa-6,10-dithia-3,13-diazacyclo-
tetradecane(chloro)cobalt(III) triperchlorate trihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 109.662(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0402(3)
_cell_length_b                   32.169(1)
_cell_length_c                   11.8590(4)
_cell_measurement_reflns_used    6887
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.22
_cell_volume                     2888.43(17)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;
ORTEP-III (Burnett & Johnson, 1996), KRYSTAL
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement
;
modified ORFLS (Busing, Martin & Levy, 1962), KRYSTAL
;
_computing_structure_solution
;
SIR97 (Cascarano et al., 1996), KRYSTAL (Hazell, 1995)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23467
_diffrn_reflns_reduction_process 23467
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.9055
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (Siemens, 1995)'
_exptl_crystal_colour            'Dark red-blue'
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       rod
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.2(2)
_refine_diff_density_min         -0.7(2)
_refine_ls_extinction_coef       30(13)
_refine_ls_extinction_method
;
B-C type 1
Lorentzian isotropic (Becker & Coppens, 1974)
;
_refine_ls_goodness_of_fit_obs   1.29
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5891
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.064
_refine_ls_shift/su_max          0.0521
_refine_ls_shift/su_mean         0.0085
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.064
_reflns_number_observed          5891
_reflns_number_total             7461
_reflns_observed_criterion       I>4\s(I)
_cod_data_source_file            b205832d.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 40 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^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~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2888.4(2)
_cod_database_code               7011918