Structural, Conformational, and Spectroscopic Studies of Primary Amine Complexes of Iron(II) Porphyrins
Orde Q. Munro; P. Sizwe Madlala; Richard A. F. Warby; Takele B. Seda; Giovanni Hearne; Inorganic Chemistry 38 (1999) 4724–4736; doi:10.1021/ic990178q

data_4322302
_publ_section_title
;
 Structural, Conformational, and Spectroscopic Studies of Primary Amine
 Complexes of Iron(II) Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4724
_journal_page_last               4736
_journal_paper_doi               10.1021/ic990178q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C58 H46 Fe N6'
_chemical_formula_weight         882.86
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.69(3)
_cell_angle_beta                 101.97(3)
_cell_angle_gamma                112.16(4)
_cell_formula_units_Z            2
_cell_length_a                   11.742(5)
_cell_length_b                   12.348(6)
_cell_length_c                   17.404(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     2222.7(18)
_computing_cell_refinement
'Structure Determination Program (B.A. Frenz & Assoc. & Enraf Nonius)'
_computing_data_collection
'Structure Determination Program (B.A. Frenz & Assoc. & Enraf Nonius)'
_computing_data_reduction
'Structure Determination Program (B.A. Frenz & Assoc. & Enraf Nonius)'
_computing_molecular_graphics    'ORTEX6a (P. McArdle, UCG, Ireland, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       Omega-2Theta
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6878
_diffrn_reflns_theta_full        22.97
_diffrn_reflns_theta_max         22.97
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count '60 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.9442
_exptl_absorpt_correction_T_min  0.8764
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       'Eight-sided rhomb'
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         6159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0271P)^2^+3.8246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                4702
_reflns_number_total             6159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990178q_2.cif
_cod_data_source_block           sm01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+3.8246P] 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^)+(0.0271P)^2^+3.8246P] 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        2222.7(15)
_cod_database_code               4322302