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_4130190
_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
'C30 H24 N4 O10 Pd2, C30 H25 N4 O10 Pd2, 6(C H Cl3), 0.5(C6 H14)'
_chemical_formula_sum            'C69 H62 Cl18 N8 O20 Pd4'
_chemical_formula_weight         2386.96
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2012-12-04
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                89.68(2)
_cell_angle_beta                 85.150(17)
_cell_angle_gamma                66.57(3)
_cell_formula_units_Z            2
_cell_length_a                   12.919(4)
_cell_length_b                   14.743(5)
_cell_length_c                   25.813(12)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.23
_cell_volume                     4493(3)
_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      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62947
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.550
_diffrn_reflns_theta_min         1.584
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.509
_refine_diff_density_min         -1.889
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         18315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+21.4763P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13111
_reflns_number_total             18315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b01188_si_002.cif
_cod_data_source_block           Structure-B
_cod_database_code               4130190
_diffrn_reflns_sigmai/neti       0.0956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H11 of C11, H14 of C14, H10 of C10, H9 of C9, H12 of C12, H20 of C20, H13
  of C13, H21 of C21, H3 of C3, H1 of C1, H22 of C22, H2 of C2, {H10B,H10C} of
  C10S, {H9SA,H9SB} of C9S, {H8SA,H8SB} of C8S, H5S of C5S, H4S of C4S, {H11B,
  H11C} of C11S, H12A of C12A, H2A of C2A, H9A of C9A, H11A of C11A, H14A of
  C14A, H21A of C21A, H22A of C22A, H13A of C13A, H4A of N4A, H20A of C20A, H3A
  of C3A, H10A of C10A, H1A of C1A, H3S of C3S, H6S of C6S, H2S of C2S, H1S of
  C1S
 At 1.5 times of:
  {H30D,H30E,H30F} of C30, {H26D,H26E,H26F} of C26, {H28D,H28E,H28F} of C28,
  {H24D,H24E,H24F} of C24, {H7SA,H7SB,H7SC} of C7S, {H12B,H12C,H12D} of C12S,
  {H30A,H30B,H30C} of C30A, {H28A,H28B,H28C} of C28A, {H26A,H26B,H26C} of C26A,
  {H24A,H24B,H24C} of C24A
2. Others
 Fixed Sof: C7S(0.5) H7SA(0.5) H7SB(0.5) H7SC(0.5) C8S(0.5) H8SA(0.5)
 H8SB(0.5) C9S(0.5) H9SA(0.5) H9SB(0.5) C10S(0.5) H10B(0.5) H10C(0.5) C11S(0.5)
 H11B(0.5) H11C(0.5) C12S(0.5) H12B(0.5) H12C(0.5) H12D(0.5)
 Fixed Uiso: C7S(0.1362) C8S(0.1362) C9S(0.1362) C10S(0.1362) C11S(0.1362)
 C12S(0.1362)
3.a Free rotating group:
 C7S(C8S,C9S,C10S,C11S,C12S)
3.b Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S), C6S(H6S), C3S(H3S), C4S(H4S), C5S(H5S)
3.c Secondary CH2 refined with riding coordinates:
 C8S(H8SA,H8SB), C9S(H9SA,H9SB), C10S(H10B,H10C), C11S(H11B,H11C)
3.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C20(H20), C21(H21), C22(H22), N4A(H4A), C1A(H1A), C2A(H2A), C3A(H3A),
  C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A),
 C20A(H20A), C21A(H21A), C22A(H22A)
3.e Idealised Me refined as rotating group:
 C24(H24D,H24E,H24F), C26(H26D,H26E,H26F), C28(H28D,H28E,H28F), C30(H30D,H30E,
 H30F), C24A(H24A,H24B,H24C), C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C),
 C30A(H30A,H30B,H30C), C7S(H7SA,H7SB,H7SC), C12S(H12B,H12C,H12D)
;
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.807
_shelx_hkl_checksum              9869
_shelx_res_checksum              19810
_shelxl_version_number           2012-4