Synthesis and structures of transition metal pacman complexes of heteroditopic Schiff-base pyrrole macrocycles.
Leeland, James W.; Finn, Colin; Escuyer, Bérengère; Kawaguchi, Hiroyuki; Nichol, Gary S.; Slawin, Alexandra M. Z.; Love, Jason B.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 13815–13831; doi:10.1039/c2dt31850d

data_7020554
_publ_section_title
;
 Synthesis and structures of transition metal pacman complexes of
 heteroditopic Schiff-base pyrrole macrocycles.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13815
_journal_page_last               13831
_journal_paper_doi               10.1039/c2dt31850d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C32 H35 N5 O2 Pd'
_chemical_formula_weight         628.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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-2012
_cell_angle_alpha                90
_cell_angle_beta                 91.0660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.7164(9)
_cell_length_b                   23.209(2)
_cell_length_c                   25.187(3)
_cell_measurement_reflns_used    16369
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.471
_cell_measurement_theta_min      1.9323
_cell_volume                     5678.9(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_device_type  'Rigaku Mercury diffractometer'
_diffrn_measurement_method       'phi or omega oscillation scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            43926
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.840
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.523
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         15119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0735P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12143
_reflns_number_total             15119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c2dt31850d.txt
_cod_data_source_block           lppd_pdlnme
_cod_database_code               7020554
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.874
_diffrn_reflns_sigmai/neti       0.0410
_shelxl_version_number           2012-4