Self-Assembly of Palladium-Based Macrocycles with N-Heterocyclic Carbene as the “Corner” Ligand†
Xiao, Xu-Qiong; Jia, Ai-Quan; Lin, Yue-Jian; Jin, Guo-Xin; Organometallics 29 (2010) 4842–; doi:10.1021/om100040g

data_4065633
_publ_section_title
;
 Self-Assembly of Palladium-Based Macrocycles with N-Heterocyclic Carbene
 as the &#x201C;Corner&#x201D; Ligand&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4842
_journal_paper_doi               10.1021/om100040g
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C78 H80 F12 N12 O12 Pd2 S8'
_chemical_formula_weight         2074.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.167(14)
_cell_length_b                   20.65(2)
_cell_length_c                   38.82(4)
_cell_measurement_reflns_used    903
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.912
_cell_measurement_theta_min      2.320
_cell_volume                     10555(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1846
_diffrn_reflns_av_sigmaI/netI    0.3523
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            37297
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.12
_diffrn_standards_decay_%        9.95
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.9555
_exptl_absorpt_correction_T_min  0.9187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.818
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         18573
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.2130
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1930
_reflns_number_gt                5266
_reflns_number_total             18573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100040g_si_001.cif
_cod_data_source_block           Complex6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        10556(19)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4065633