Synthesis, structural characterization and anion binding studies of palladium macrocycles with hydrogen-bonding ligands.
Diaz, Pilar; Tovilla, Jorge A.; Ballester, Pablo; Benet-Buchholz, Jordi; Vilar, Ramón; Dalton transactions (Cambridge, England : 2003)  (2007) 3516–3525; doi:10.1039/b703660d

data_7005620
_publ_section_title
;
 Synthesis, structural characterization and anion binding studies of
 palladium macrocycles with hydrogen-bonding ligands.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3516
_journal_page_last               3525
_journal_paper_doi               10.1039/b703660d
_journal_year                    2007
_chemical_formula_sum            'C100.25 H94.5 F12 N8 O18.75 P4 Pd2 S4'
_chemical_formula_weight         2404.26
_chemical_name_systematic
;

?

;
_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_method           SHELXL-97
_cell_angle_alpha                95.680(2)
_cell_angle_beta                 94.482(2)
_cell_angle_gamma                104.570(2)
_cell_formula_units_Z            2
_cell_length_a                   15.8443(7)
_cell_length_b                   18.8383(9)
_cell_length_c                   20.6983(8)
_cell_measurement_temperature    153(2)
_cell_volume                     5915.8(5)
_computing_cell_refinement       'Bruker SAINT program vers. 5.0'
_computing_data_collection       'Bruker Smart CCDC area detector system'
_computing_data_reduction        'Bruker SAINT program vers. 5.0'
_computing_molecular_graphics    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_publication_material  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            'Smart 1000 CCD area detector'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'four-circle diffractometer Bruker P4'
_diffrn_measurement_method
;
Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1251
_diffrn_reflns_av_sigmaI/netI    0.1867
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74819
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         0.99
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           240
_diffrn_source_power             40
_diffrn_source_size              '10 mm x 0.5 mm fine focus'
_diffrn_source_type              'MACScience Co. M18X-HF'
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.873952
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Version 2.1 2003 Bruker-Nonius
Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.423
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1404
_refine_ls_number_reflns         28010
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1796
_refine_ls_R_factor_gt           0.0841
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2237
_refine_ls_wR_factor_ref         0.2690
_reflns_number_gt                12427
_reflns_number_total             28010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b703660d.txt
_cod_data_source_block           pd210isg
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5915.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C100.25 H94.50 F12 N8 O18.75 P4 Pd2 S4'
_cod_database_code               7005620