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_4319903
_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         'C60 H50 Co F6 N6 Sb'
_chemical_formula_sum            'C60 H50 Co F6 N6 Sb'
_chemical_formula_weight         1149.74
_chemical_melting_point          ?
_chemical_name_common            '[Co(TPP)(PhCH2CH2NH2)2]SbF6'
_chemical_name_systematic
; 
bis(phenethylamine)(5,10,15,20-mesotetraphenylporphinato)cobalt(III)
hexafluoroantimonate(V)  
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 94.2140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6378(5)
_cell_length_b                   22.0466(11)
_cell_length_c                   10.9585(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      2
_cell_volume                     2563.1(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28353
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         5.56
_diffrn_standards_decay_%        'No detectable decay'
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.7701
_exptl_absorpt_correction_T_min  0.7100
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   None
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Irregular rhomb'
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.524(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         12360
_refine_ls_number_restraints     389
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.689
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+2.2464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                11393
_reflns_number_total             12360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000976c_3.cif
_cod_data_source_block           scs3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'Not measured' 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 'Monoclinic' changed to 'monoclinic'
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 
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_cod_database_code               4319903