Equipping metallo-supramolecular macrocycles with functional groups: assemblies of pyridine-substituted urea ligands.
Troff, Ralf W.; Hovorka, Rainer; Weilandt, Torsten; Lützen, Arne; Cetina, Mario; Nieger, Martin; Lentz, Dieter; Rissanen, Kari; Schalley, Christoph A.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 8410–8420; doi:10.1039/c2dt30190c

data_7019340
_publ_section_title
;
 Equipping metallo-supramolecular macrocycles with functional groups:
 assemblies of pyridine-substituted urea ligands.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8410
_journal_page_last               8420
_journal_paper_doi               10.1039/c2dt30190c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
'C80 H80 N8 O2 P4 Pd2 4+, 4(C F3 O3 S 1-), 3(C3 H7 N O), 1/2(C4 H10 O), H2 O'
_chemical_formula_sum            'C95 H108 F12 N11 O18.5 P4 Pd2 S4'
_chemical_formula_weight         2392.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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-97
_cell_angle_alpha                87.680(1)
_cell_angle_beta                 78.927(1)
_cell_angle_gamma                71.110(1)
_cell_formula_units_Z            2
_cell_length_a                   16.3896(2)
_cell_length_b                   18.3213(2)
_cell_length_c                   21.5285(3)
_cell_measurement_reflns_used    21254
_cell_measurement_temperature    173.0(1)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.407
_cell_volume                     6000.88(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Apex II Diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.579874E-1
_diffrn_orient_matrix_UB_12      -0.126827E-1
_diffrn_orient_matrix_UB_13      -0.296163E-1
_diffrn_orient_matrix_UB_21      0.300837E-1
_diffrn_orient_matrix_UB_22      -0.35301E-2
_diffrn_orient_matrix_UB_23      0.367946E-1
_diffrn_orient_matrix_UB_31      0.67559E-2
_diffrn_orient_matrix_UB_32      -0.56182E-1
_diffrn_orient_matrix_UB_33      0.32375E-2
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            71355
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.67
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. SADABS 2008/2; University of G\"ottingen: G\"ottingen,
Germany, 2008.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2454
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.761
_refine_diff_density_min         -2.813
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1317
_refine_ls_number_reflns         21076
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2499
_refine_ls_wR_factor_ref         0.2707
_reflns_number_gt                16013
_reflns_number_total             21076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30190c.txt
_cod_data_source_block           25a
_cod_original_cell_volume        6000.9(1)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C95 H108 F12 N11 O18.50 P4 Pd2 S4'
_cod_database_code               7019340