Bidentate cycloimidate palladium complexes with aliphatic and aromatic anagostic bonds
Stephan Scholer; Maike H. Wahl; Nicole I. C. Wurster; Arik Puls; Christof Hattig; Gerald Dyker; Chem.Commun. 50 (2014) 5909–; doi:10.1039/C4CC01060D

data_7113410
_publ_section_title
;
 Bidentate cycloimidate palladium complexes with aliphatic and aromatic
 anagostic bonds
;
_journal_name_full               Chem.Commun.
_journal_page_first              5909
_journal_paper_doi               10.1039/C4CC01060D
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C36 H32 Cl2 N2 O4 Pd'
_chemical_formula_sum            'C36 H32 Cl2 N2 O4 Pd'
_chemical_formula_weight         733.93
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-11-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.11.13 svn.r2834 for OlexSys, GUI svn.r4705)
;
_cell_angle_alpha                90
_cell_angle_beta                 77.5137(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.08922(16)
_cell_length_b                   15.4848(2)
_cell_length_c                   21.0438(3)
_cell_measurement_reflns_used    7000
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.463
_cell_measurement_theta_min      2.740
_cell_volume                     3209.90(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.39 (release 18-08-2010 CrysAlis171 .NET)
(compiled Aug 18 2010,17:42:00)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.39 (release 18-08-2010 CrysAlis171 .NET)
(compiled Aug 18 2010,17:42:00)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.39 (release 18-08-2010 CrysAlis171 .NET)
(compiled Aug 18 2010,17:42:00)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41281
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.899
_diffrn_reflns_theta_min         3.159
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.39 (release 18-08-2010 CrysAlis171 .NET)
(compiled Aug 18 2010,17:42:00)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 6398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.025(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         14829
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.7960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                14286
_reflns_number_total             14829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc01060d2.cif
_cod_data_source_block           ssANW20
_cod_depositor_comments
;
2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C72 H64 Cl4 N4 O8 Pd2'
_cod_original_formula_weight         1467.87
_cod_original_formula_moiety         '2(C36 H32 Cl2 N2 O4 Pd)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3209.91(8)
_cod_database_code               7113410
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23), C23A(H23A)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C30(H30A,H30B), C24A(H24C,H24D), C30A(H30C,H30D)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C26(H26), C13(H13), C4(H4), C5(H5), C3(H3), C20(H20),
 C19(H19), C17(H17), C10(H10), C11(H11), C14(H14), C27(H27), C28(H28), C29(H29),
  C36(H36), C35(H35), C34(H34), C33(H33), C32(H32), C5A(H5A), C29A(H29A),
 C34A(H34A), C3A(H3A), C11A(H11A), C14A(H14A), C36A(H36A), C19A(H19A),
 C13A(H13A), C35A(H35A), C17A(H17A), C26A(H26A), C16A(H16A), C4A(H4A),
 C10A(H10A), C28A(H28A), C27A(H27A), C32A(H32A), C33A(H33A), C20A(H20A),
 C6A(H6A)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C21A(H21D,H21E,H21F), C22A(H22D,
 H22E,H22F)
;