Five- to Six-Coordination in (Nitrosyl)iron(II) Porphyrinates: Effects of Binding the Sixth Ligand
Graeme R. A. Wyllie; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 42 (2003) 5722–5734; doi:10.1021/ic034473t

data_4314192
_publ_section_title
;
 Five- to Six-Coordination in (Nitrosyl)iron(II) Porphyrinates: Effects of
 Binding the Sixth Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5722
_journal_page_last               5734
_journal_paper_doi               10.1021/ic034473t
_journal_volume                  42
_journal_year                    2003
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C48 H34 Fe N7 O, C H Cl3'
_chemical_formula_sum            'C49 H35 Cl3 Fe N7 O'
_chemical_formula_weight         900.04
_chemical_melting_point          ?
_chemical_name_common            '[Fe(TPP)(NO)(1-MeIm)].CHCl3'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   17.5274(8)
_cell_length_b                   25.2009(11)
_cell_length_c                   9.6227(4)
_cell_measurement_reflns_used    6388
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.257
_cell_measurement_theta_min      2.415
_cell_volume                     4250.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTl'
_computing_molecular_graphics    'ORTEP III (Burnett, Johnson, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            46920
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        'no measureable decay'
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.451(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         10522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                9046
_reflns_number_total             10522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034473tsi20030505_025109_2.cif
_cod_data_source_block           tpp1meim
_cod_depositor_comments
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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:

'_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 
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_cod_database_code               4314192