Dithiacrown Ether Substituted Porphyrazines: Synthesis, Single-Crystal Structure, and Control of Aggregation in Solution by Complexation of Transition-Metal Ions
Cornelus F. van Nostrum; Franciscus B. G. Benneker; Hugo Brussaard; Huub Kooijman; Nora Veldman; Anthony L. Spek; Joop Schoonman; Martinus C. Feiters; Roeland J. M. Nolte; Inorganic Chemistry 35 (1996) 959–969; doi:10.1021/ic950704n

data_4323781
_publ_section_title
;
 Dithiacrown Ether Substituted Porphyrazines: Synthesis, Single-Crystal
 Structure, and Control of Aggregation in Solution by Complexation of
 Transition-Metal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              959
_journal_page_last               969
_journal_paper_doi               10.1021/ic950704n
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C56 H82 Mg N8 O17 S8'
_chemical_formula_weight         1420.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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
_cell_angle_alpha                84.904(14)
_cell_angle_beta                 85.21(2)
_cell_angle_gamma                89.29(2)
_cell_formula_units_Z            2
_cell_length_a                   9.584(3)
_cell_length_b                   17.672(2)
_cell_length_c                   19.620(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3298.3(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1501
_diffrn_reflns_av_sigmaI/netI    0.1572
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8948
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.353
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_F_000             1500
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.161
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         8603
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.1771
_refine_ls_R_factor_obs          0.0839
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0753P)^2^+12.0473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2228
_refine_ls_wR_factor_obs         0.1704
_reflns_number_observed          4457
_reflns_number_total             8608
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950704n_2.cif
_cod_data_source_block           S875A
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0753P)^2^+12.0473P] 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^)+( 0.0753P)^2^+12.0473P]
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        3298.4(14)
_cod_database_code               4323781