Synthesis and Physicochemical Characterization of Protonated and Deprotonated Forms in Heteroleptic Lanthanide(III) Porphyrinate Double-Deckers. X-ray Structure of GdIIIH(oep)(tpp) at 298 and 21 K
Georgios A. Spyroulias; Catherine P. Raptopoulou; Dominique de Montauzon; Alain Mari; René Poilblanc; Aris Terzis; Athanassios G. Coutsolelos; Inorganic Chemistry 38 (1999) 1683–1696; doi:10.1021/ic970879s

data_4321896
_publ_section_title
;
 Synthesis and Physicochemical Characterization of Protonated and
 Deprotonated Forms in Heteroleptic Lanthanide(III) Porphyrinate
 Double-Deckers. X-ray Structure of GdIIIH(oep)(tpp) at 298 and 21 K
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1683
_journal_page_last               1696
_journal_paper_doi               10.1021/ic970879s
_journal_volume                  38
_journal_year                    1999
_chemical_formula_analytical     '[(tpp)Hoep)Gd].Ch2Cl2'
_chemical_formula_structural     '[(C44 H28 N4)(C36 H45 N4)Gd].2CH2Cl2'
_chemical_formula_sum            'C81 H75 Cl2 Gd N8'
_chemical_formula_weight         1388.64
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.938(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.779(1)
_cell_length_b                   19.410(1)
_cell_length_c                   26.183(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5.5
_cell_volume                     6851.2(8)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8638
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        -2.7%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  1.24
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_meas      1.33
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.098
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     828
_refine_ls_number_reflns         8362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.255
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_obs          0.0474
_refine_ls_shift/esd_max         -0.405
_refine_ls_shift/esd_mean        0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+21.3074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1463
_refine_ls_wR_factor_obs         0.1149
_reflns_number_observed          6589
_reflns_number_total             8413
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970879s_1.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+21.3074P] 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^)+(0.0294P)^2^+21.3074P] 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        6851.5(8)
_cod_database_code               4321896