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_4322301
_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            'C52 H50 Fe N6'
_chemical_formula_weight         814.83
_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                94.15(4)
_cell_angle_beta                 105.62(5)
_cell_angle_gamma                113.88(6)
_cell_formula_units_Z            1
_cell_length_a                   10.118(10)
_cell_length_b                   11.086(14)
_cell_length_c                   11.205(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     1083.1(19)
_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    'ORTEX 7e (P. McArdle, UCG, Ireland, 1999)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            4840
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        'no significant decay'
_diffrn_standards_interval_count '60 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.9329
_exptl_absorpt_correction_T_min  0.8498
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            Purple-black
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Six-sided rhomb'
_exptl_crystal_F_000             430
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0446P)^2^+0.5755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                3193
_reflns_number_total             3786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990178q_1.cif
_cod_data_source_block           raw1a
_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^)+(0.0446P)^2^+0.5755P] 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^)+(0.0446P)^2^+0.5755P] 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        1083.1(18)
_cod_database_code               4322301