Structurally Diverse Diazafluorene-Ligated Palladium(II) Complexes and Their Implications for Aerobic Oxidation Reactions.
White, Paul B.; Jaworski, Jonathan N.; Fry, Charles G.; Dolinar, Brian S.; Guzei, Ilia A.; Stahl, Shannon S.; Journal of the American Chemical Society 138 (2016) 4869–4880; doi:10.1021/jacs.6b01188

data_4130191
_publ_section_title
;
 Structurally Diverse Diazafluorene-Ligated Palladium(II) Complexes and
 Their Implications for Aerobic Oxidation Reactions.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4869
_journal_page_last               4880
_journal_paper_doi               10.1021/jacs.6b01188
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C26 H18 N4 O6 Pd, 2(C H Cl3)'
_chemical_formula_sum            'C28 H20 Cl6 N4 O6 Pd'
_chemical_formula_weight         827.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2012-10-12
_audit_creation_method
;
  Olex2 1.2-dev
  (compiled Oct  2 2012 15:48:42, GUI svn.r4353)
;
_cell_angle_alpha                73.333(5)
_cell_angle_beta                 88.112(7)
_cell_angle_gamma                88.791(6)
_cell_formula_units_Z            1
_cell_length_a                   5.9835(5)
_cell_length_b                   10.4400(9)
_cell_length_c                   12.697(2)
_cell_measurement_reflns_used    6660
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.566
_cell_measurement_theta_min      3.635
_cell_volume                     759.36(15)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12291
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.085
_diffrn_reflns_theta_min         3.635
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.231
_exptl_absorpt_correction_T_max  0.7660
_exptl_absorpt_correction_T_min  0.4588
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
? was used for absorption correction.
wR2(int) was 0.0586 before and 0.0345 after correction.
The Ratio of minimum to maximum transmission is 0.5990.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.4722P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2686
_reflns_number_total             2820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b01188_si_002.cif
_cod_data_source_block           Structure-E
_cod_original_cell_volume        759.35(15)
_cod_database_code               4130191
_diffrn_reflns_sigmai/neti       0.0194
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H8 of C8, H9 of C9, H14 of C14, H3 of C3, H7 of C7, H1 of C1, H2 of C2
 At 1.5 times of:
  {H13A,H13B,H13C} of C13
2.a Ternary CH refined with riding coordinates:
 C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.304
_shelx_hkl_checksum              46192
_shelx_res_checksum              69610
_shelxl_version_number           2012-4