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_7110369
_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            'C49 H59 B Co N4 O2'
_chemical_formula_weight         805.74
_chemical_name_systematic
; 
(1-carboxymethyl-4-methylene-1,4,8,11-tetraazacyclotetradecane)
-cobalt (III) percholorate
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.2770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8555(5)
_cell_length_b                   17.4488(6)
_cell_length_c                   17.2455(6)
_cell_measurement_reflns_used    9620
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.33
_cell_volume                     4193.2(3)
_computing_cell_refinement       'Siemens SMART (Siemens, 1994a)'
_computing_data_collection       'Siemens SMART (Siemens, 1994a)'
_computing_data_reduction        'Siemens SHELXTL (Siemens, 1994b)'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       \w
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25441
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.8834
_exptl_absorpt_correction_T_min  0.8048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+2.9123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1492
_reflns_number_gt                6384
_reflns_number_total             8199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            807365asup1.cif
_cod_data_source_block           dmt15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0746P)^2^+2.9123P] 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^)+(0.0746P)^2^+2.9123P] 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        4193.2(2)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7110369