"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_4323879
_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            'C16 H32 Cl2 N6 O14 Pd'
_chemical_formula_weight         709.78
_chemical_name_common            '[Pd(dino[18]mac)](ClO~4~)~2~'
_chemical_name_systematic
;(3,12-Dimethyl-3,12-dinitro-1,5,10,14-tetraazacyclooctadecane)palladium(II) 
 perchlorate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_date             96-04-03
_audit_creation_method           SHELXL
_cell_angle_alpha                91.76(6)
_cell_angle_beta                 101.73(7)
_cell_angle_gamma                112.83(5)
_cell_formula_units_Z            2
_cell_length_a                   7.746(5)
_cell_length_b                   9.912(5)
_cell_length_c                   18.96(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     1303.9(19)
_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
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    56.0267
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4595
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        1.03
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.83
_exptl_crystal_colour            near-colourless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_meas      1.82
_exptl_crystal_density_method    flotation
_exptl_crystal_description       plate
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.119
_refine_diff_density_min         -1.734
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_obs          0.0713
_refine_ls_shift/esd_max         -0.109
_refine_ls_shift/esd_mean        0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1337P)^2^+5.5100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2149
_refine_ls_wR_factor_obs         0.2061
_reflns_number_observed          3921
_reflns_number_total             4595
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951628r_3.cif
_cod_data_source_block           (III)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1337P)^2^+5.5100P] 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^)+(0.1337P)^2^+5.5100P] 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        1303.9(11)
_cod_database_code               4323879