From discrete monomeric complexes to hydrogen-bonded dimeric assemblies based on sterically encumbered square planar palladium(II) ONN-pincers.
Adeyi, Okoh; Cross, Warren B.; Forrest, Gregory; Godfrey, Luke; Hope, Eric G.; McLeod, Andrew; Singh, Amandeep; Singh, Kuldip; Solan, Gregory A.; Wang, Yining; Wright, Luka A.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7710–7723; doi:10.1039/c3dt50176k

data_7022863
_publ_section_title
;
 From discrete monomeric complexes to hydrogen-bonded dimeric assemblies
 based on sterically encumbered square planar palladium(II) ONN-pincers.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7710
_journal_page_last               7723
_journal_paper_doi               10.1039/c3dt50176k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C33 H36 N2 O3 Pd,C H Cl3,3(C6 H14) '
_chemical_formula_sum            'C52 H79 Cl3 N2 O3 Pd'
_chemical_formula_weight         992.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.655(6)
_cell_angle_beta                 115.655(6)
_cell_angle_gamma                115.655(6)
_cell_formula_units_Z            6
_cell_length_a                   22.469(7)
_cell_length_b                   22.469(7)
_cell_length_c                   22.469(7)
_cell_measurement_reflns_used    603
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.370
_cell_measurement_theta_min      2.174
_cell_volume                     5952(4)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex 2000 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  0.3336
_diffrn_reflns_av_sigmaI/netI    0.3312
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46610
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 3153 reflections(SADABS);Rint 0.2032 before
correction and 0.1767 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Disordered CHCl3 and C6H14 were omitted using the SQUEEZE option of PLATON.
The solvent accessible voids are 2022.3 3 with an estimated 1275e/cell to
be added. Six solvent CHCl3 and eighteen C6H14 molecules/unit cell
accounting for 1248e were included in the formula, FWt, (000) and density
calculations. PLATON Reference:Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_refine_diff_density_max         0.565
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7800
_refine_ls_number_restraints     351
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.1881
_refine_ls_R_factor_gt           0.0781
_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^)+(0.0403P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                3035
_reflns_number_total             7800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50176k.txt
_cod_data_source_block           10081
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5952(3)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7022863