Decarboxylation of an α-amino acid coordinated to cobalt(iii): kinetic stabilisation and molecular structure of a Co‒C‒N three-membered ring incorporated into a cobalt(iii) macrocyclic ligand complex†‡
Tonei, Deborah M.; Baker, Lisa-Jane; Brothers, Penelope J.; Clark, George R.; Ware, David C.; Chemical Communications  (1998) 2593–; doi:10.1039/a807365a

data_7110370
_publ_section_title
;
 Decarboxylation of an \a-amino acid coordinated to cobalt(iii): kinetic
 stabilisation and molecular structure of a Co--C--N three-membered ring
 incorporated into a cobalt(iii) macrocyclic ligand
 complex&#x2020;&#x2021;
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2593
_journal_paper_doi               10.1039/a807365a
_journal_year                    1998
_chemical_formula_sum            'C13 H25 Cl2 Co N4 O6'
_chemical_formula_weight         463.20
_chemical_name_systematic
; 
chloro(1-carboxymethyl-4-methyl-1,4,8,11-tetraazacyclotetradecane)-
cobalt (III) perchlorate 
;
_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
_cell_angle_alpha                90.95(3)
_cell_angle_beta                 109.51(3)
_cell_angle_gamma                96.09(2)
_cell_formula_units_Z            2
_cell_length_a                   8.456(2)
_cell_length_b                   9.689(3)
_cell_length_c                   12.161(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      14.22
_cell_measurement_theta_min      11.45
_cell_volume                     932.4(6)
_computing_cell_refinement       'CAD-4 Software (Enraf, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf, 1989)'
_computing_data_reduction        'Local Program'
_computing_molecular_graphics    'Siemens SHELXTL (Siemens,1994b)'
_computing_publication_material  'Siemens SHELXTL (Siemens,1994b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3323
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al, 1968)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+1.9598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                2561
_reflns_number_total             3188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            807365asup1.cif
_cod_data_source_block           dmt7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value
'w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+1.9598P] 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^)+(0.0970P)^2^+1.9598P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110370