Studies of Iron(III) Porphyrinates Containing Silanethiolate Ligands
Daniel J. Meininger; Jonathan D. Caranto; Hadi D. Arman; Zachary J. Tonzetich; Inorganic Chemistry 52 (2013) 12468–12476; doi:10.1021/ic401467k

data_4336561
_publ_contact_author_address
;
    Department of Chemistry,
    The University of Texas,
    One UTSA Circle,
    San Antonio, Texas 78249-0698,
    U.S.A.
;
_publ_contact_author_email
;
hadi.arman@utsa.edu
;
_publ_section_title
;
 Studies of Iron(III) Porphyrinates Containing Silanethiolate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12468
_journal_page_last               12476
_journal_paper_doi               10.1021/ic401467k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C74 H67 Fe N4 S Si, 0.8(C H2 Cl2)'
_chemical_formula_sum            'C74.8 H68.6 Cl1.6 Fe N4 S Si'
_chemical_formula_weight         1196.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.668(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4254(13)
_cell_length_b                   18.9508(14)
_cell_length_c                   22.8901(19)
_cell_measurement_reflns_used    20068
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6750.2(10)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1255
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9440
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        23.10
_diffrn_reflns_theta_max         23.10
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       needle
_exptl_crystal_F_000             2514
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         9440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.1982
_reflns_number_gt                5585
_reflns_number_total             9440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401467k_si_002_3.cif
_cod_data_source_block           '[Fe(SSiPh3)(TMP)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'const' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        6750.2(9)
_cod_original_formula_sum        'C74.80 H68.60 Cl1.60 Fe N4 S Si'
_cod_database_code               4336561