Structural, Computational, and 59Co NMR Studies of Primary and Secondary Amine Complexes of Co(III) Porphyrins
Orde Q. Munro; Sibongiseni C. Shabalala; Nicola J. Brown; Inorganic Chemistry 40 (2001) 3303–3317; doi:10.1021/ic000976c

data_4319901
_publ_section_title
;
 Structural, Computational, and 59Co NMR Studies of Primary and Secondary
 Amine Complexes of Co(III) Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3303
_journal_page_last               3317
_journal_paper_doi               10.1021/ic000976c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C52 H50 Co F6 N6 Sb'
_chemical_formula_sum            'C52 H50 Co F6 N6 Sb'
_chemical_formula_weight         1053.66
_chemical_melting_point          ?
_chemical_name_common            '[Co(TPP)(1-BuNH2)2]SbF6'
_chemical_name_systematic
; 
bis(1-butylamine)(5,10,15,20-mesotetraphenylporphinato)cobalt(III)
hexafluoroantimonate(V) 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2614(9)
_cell_length_b                   12.7546(7)
_cell_length_c                   23.2873(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      2
_cell_volume                     4830.0(5)
_computing_cell_refinement       SAINT
_computing_data_collection       SAINT
_computing_data_reduction        SAINT
_computing_molecular_graphics    'OSCAIL 8 (P. McArdle, 1999)'
_computing_publication_material  'ORTEP32 (L. J. Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'SIEMENS SMART 1000'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            46199
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         5.55
_diffrn_standards_decay_%        'No significant decay'
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.8300
_exptl_absorpt_correction_T_min  0.5944
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   None
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Plate-like rhomb'
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5947
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+7.7178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                4579
_reflns_number_total             5947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000976c_1.cif
_cod_data_source_block           scs2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'Not determined' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4319901