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_7113412
_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         'C54 H58 Cl4 N2 O8 Pd2, 2(C H2 Cl2)'
_chemical_formula_sum            'C56 H62 Cl8 N2 O8 Pd2'
_chemical_formula_weight         1387.47
_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     direct
_audit_creation_date             2014-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1682(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.80633(12)
_cell_length_b                   13.99186(13)
_cell_length_c                   22.0766(2)
_cell_measurement_reflns_used    1200
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      73.522
_cell_measurement_theta_min      4.873
_cell_volume                     3021.09(5)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      106.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29992
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.651
_diffrn_reflns_theta_min         3.743
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.485
_exptl_absorpt_correction_T_max  0.507
_exptl_absorpt_correction_T_min  0.415
_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    1.525
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 4828 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.028(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         11595
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0602P)^2^+2.1883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.941
_reflns_Friedel_fraction_max     0.885
_reflns_number_gt                11131
_reflns_number_total             11595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc01060d2.cif
_cod_data_source_block           ssa421
_cod_original_cell_volume        3021.09(6)
_cod_database_code               7113412
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23), C24(H24), C50(H50), C51(H51)
2.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33),
  C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C46(H46), C47(H47)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1Q(H1Q), O2(H2)
;
_shelx_res_checksum              88114
_shelx_hkl_checksum              59083
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'