A Heterobimetallic Pd‒Zn Complex: Study of a d8‒d10 Bond in Solid State, in Solution, and in Silico
Oeschger, Raphael J.; Chen, Peter; Organometallics 36 (2017) 1465–; doi:10.1021/acs.organomet.7b00113

data_4087271
_publ_section_title
;
 A Heterobimetallic Pd--Zn Complex: Study of a d8--d10 Bond in Solid
 State, in Solution, and in Silico
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1465
_journal_paper_doi               10.1021/acs.organomet.7b00113
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C38 H16 F10 N2 Pd Zn'
_chemical_formula_sum            'C38 H16 F10 N2 Pd Zn'
_chemical_formula_weight         862.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.2580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.5966(4)
_cell_length_b                   39.7673(15)
_cell_length_c                   13.4976(5)
_cell_measurement_reflns_used    9256
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.57
_cell_volume                     6082.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Bruker/Nonius Kappa Apex2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'double mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23798
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.024
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms high brilliance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  0.7340
_exptl_absorpt_correction_T_min  0.6998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0698 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.9534.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0252P)^2^+4.8800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7610
_reflns_number_total             9241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00113_si_003.cif
_cod_data_source_block           c031116_1_1_0ma
_cod_database_code               4087271
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.843
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C13(H13), C15(H15), C16(H16), C22(H22), C25(H25), C27(H27),
 C28(H28), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
;
_shelx_res_checksum              8719
_shelx_hkl_checksum              16722
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-11-03
_olex2_date_sample_submission    2016-11-03
_olex2_submission_original_sample_id c031116_1_1
_olex2_submission_special_instructions 'No special instructions were received'