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_4319904
_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         'C54 H52 Co F6 N8 O Sb'
_chemical_formula_sum            'C54 H52 Co F6 N8 O Sb'
_chemical_formula_weight         1123.72
_chemical_melting_point          ?
_chemical_name_common            '[Co(TPP)(1-MePipz)2]SbF6'
_chemical_name_systematic
; 
bis(1-methylpiperazine)(5,10,15,20-mesotetraphenylporphinato)cobalt(III) 
hexafluoroantimonate(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.2450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4112(9)
_cell_length_b                   19.0611(12)
_cell_length_c                   19.6630(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      2
_cell_volume                     5018.4(6)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0868
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50381
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         5.63
_diffrn_standards_decay_%        'No measurable decay'
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.8344
_exptl_absorpt_correction_T_min  0.5204
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   None
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.541
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12264
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1547
_refine_ls_R_factor_gt           0.0951
_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^)+(0.1558P)^2^+6.3917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2360
_refine_ls_wR_factor_ref         0.2759
_reflns_number_gt                7271
_reflns_number_total             12264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000976c_4.cif
_cod_data_source_block           scs4
_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 '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 
;
_cod_database_code               4319904