"Swollen" Macrocycles: Palladium(II)-Directed Template Syntheses of Pendant-Arm 14-, 16-, and 18-Membered Macrocycles
Monica Rossignoli; Christine C. Allen; Trevor W. Hambley; Geoffrey A. Lawrance; Marcel Maeder; Inorganic Chemistry 35 (1996) 4961–4966; doi:10.1021/ic951628r

data_4323878
_publ_contact_author
;
        Prof. Geoffrey A. Lawrance
        Department of Chemistry
        University of Newcastle
        Callaghan 2308
        Australia
;
_publ_section_title
;
 "Swollen" Macrocycles: Palladium(II)-Directed Template Syntheses of
 Pendant-Arm 14-, 16-, and 18-Membered Macrocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4961
_journal_page_last               4966
_journal_paper_doi               10.1021/ic951628r
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C14 H30 Cl2 N6 O14 Pd'
_chemical_formula_weight         683.74
_chemical_name_common            '[Pd(dino[16]mac)](ClO~4~)~2~'
_chemical_name_systematic
;
 (3,11-Dimethyl-3,11-dinitro-1,5,9,13-tetraazacyclohexadecane)palladium(II) 
 perchlorate 
;
_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                 93.18(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.391(2)
_cell_length_b                   12.816(3)
_cell_length_c                   23.925(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2568.9(13)
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction
'Enraf-Nonius Structure Determination Package'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 (Enraf-Nonius)'
_diffrn_measurement_method       \w-\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4607
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        -2.16
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.77
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_meas      1.75
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.781
_refine_ls_goodness_of_fit_obs   1.904
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.781
_refine_ls_restrained_S_obs      1.904
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_obs          0.0650
_refine_ls_shift/esd_max         0.334
_refine_ls_shift/esd_mean        0.054
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2280
_refine_ls_wR_factor_obs         0.2232
_reflns_number_observed          3815
_reflns_number_total             4492
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951628r_2.cif
_cod_data_source_block           (II)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323878