Core-Modified Porphyrin Incorporating a Phenolate Donor. Characterization of Pd(II), Ni(II), Zn(II), Cd(II), and Fe(III) Complexes
Marcin Stępień; Lechosław Latos-Grażyński; Inorganic Chemistry 42 (2003) 6183–6193; doi:10.1021/ic0345121

data_4314369
_publ_section_title
;
 Core-Modified Porphyrin Incorporating a Phenolate Donor. Characterization
 of Pd(II), Ni(II), Zn(II), Cd(II), and Fe(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6183
_journal_page_last               6193
_journal_paper_doi               10.1021/ic0345121
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C50 H29 Cl6 D2 F3 N3 O3 Pd'
_chemical_formula_weight         1097.88
_chemical_name_systematic
;
Palladium 6,11,16,21-tetraphenyl-22-hydroxybenziporphyrin
trifluoroacetic acid adduct chloroform-d disolvate
;
_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                 100.337(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9805(9)
_cell_length_b                   13.8084(7)
_cell_length_c                   22.1604(10)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_volume                     4509.6(4)
_computing_cell_refinement       'Oxford Diffraction (Poland) Sp. z o.o'
_computing_data_collection       'Oxford Diffraction (Poland) Sp. z o.o'
_computing_data_reduction        'Oxford Diffraction (Poland) Sp. z o.o'
_computing_molecular_graphics    'SHELXTL-NT V5.1, Bruker AXS 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_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       '\o scan'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29726
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         3.26
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'XPREP Ver. 5.1/NT (Bruker Analytical X-ray Systems, 1997)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10560
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.913
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+1.6742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                8664
_reflns_number_total             10560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0345121_2.cif
_cod_data_source_block           ms024a
_cod_depositor_comments
;
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.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+1.6742P] 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^)+(0.0479P)^2^+1.6742P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C50 H29 D2 Cl6 F3 N3 O3 Pd'
_cod_database_code               4314369