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_4130194
_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         'C19 H6 F12 N2 O9 Pd2, 2(C2 H F3 O2)'
_chemical_formula_sum            'C23 H8 F18 N2 O13 Pd2'
_chemical_formula_weight         1075.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-29
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.01.25 svn.r3250 for OlexSys, GUI svn.r5148)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.105(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8547(16)
_cell_length_b                   16.258(3)
_cell_length_c                   15.2201(13)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    200
_cell_measurement_theta_max      73.008
_cell_measurement_theta_min      3.484
_cell_volume                     3328.5(8)
_computing_cell_refinement       'SAINT+ Ver. 2015.9-0 (Bruker-AXS, 2015)'
_computing_data_collection       'APEX3 Ver. 2015.9-0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 2015.9-0 (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56440
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.260
_diffrn_reflns_theta_min         3.484
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_exptl_absorpt_coefficient_mu    10.303
_exptl_absorpt_correction_T_max  0.1964
_exptl_absorpt_correction_T_min  0.0728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     935
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0645P)^2^+3.3899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5648
_reflns_number_total             6565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b01188_si_002.cif
_cod_data_source_block           Structure-I
_cod_original_cell_volume        3328.5(7)
_cod_database_code               4130194
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 F4-F5 = F4-F6 = F5-F6
 2.125 with sigma of 0.02
 C17A-F7A = C17A-F8A = C17A-F9A
 1.328 with sigma of 0.001
 F7-F8 = F7-F9 = F8-F9
 2.125 with sigma of 0.02
 F7A-F8A = F7A-F9A = F8A-F9A
 2.125 with sigma of 0.02
 C2S-F1S = C2S-F2S = C2S-F3S
 1.328 with sigma of 0.001
 F1S-F2S = F1S-F3S = F2S-F3S
 2.125 with sigma of 0.02
 C4SA-F4SA = C4SA-F5SA = C4SA-F6SA
 1.328 with sigma of 0.001
 F4S-F5S = F4S-F6S = F5S-F6S
 2.125 with sigma of 0.02
 F4SA-F5SA = F4SA-F6SA = F5SA-F6SA
 2.125 with sigma of 0.02
 C15-F4 = C15-F5 = C15-F6
 1.328 with sigma of 0.001
 C17-F7 = C17-F8 = C17-F9
 1.328 with sigma of 0.001
 C4S-F4S = C4S-F5S = C4S-F6S
 1.328 with sigma of 0.001
 C15A-F4A = C15A-F5A = C15A-F6A
 1.328 with sigma of 0.001
 F4A-F5A = F4A-F6A = F5A-F6A
 2.125 with sigma of 0.02
 C2SA-F1SA = C2SA-F2SA = C2SA-F3SA
 1.328 with sigma of 0.001
 F1SA-F2SA = F1SA-F3SA = F2SA-F3SA
 2.125 with sigma of 0.02
 F10A-F11A = F10A-F12A = F11A-F12A = F10B-F11B = F10B-F12B = F11B-F12B = F10-
 F11 = F10-F12 = F11-F12
 2.125 with sigma of 0.02
 C19-F10A = C19-F11A = C19-F12A = C19-F10B = C19-F11B = C19-F12B = C19-F10 =
 C19-F11 = C19-F12
 1.328 with sigma of 0.001
 F1-F2 = F1-F3 = F2-F3 = F1A-F2A = F1A-F3A = F2A-F3A = F1B-F2B = F1B-F3B = F2B-
 F3B
 2.125 with sigma of 0.02
 C13-F1B = C13-F2B = C13-F3B = C13-F1 = C13-F2 = C13-F3 = C13-F1A = C13-F2A =
 C13-F3A
 1.328 with sigma of 0.001
 C16-F7 \\sim C16-F8 \\sim C16-F9 \\sim C16-F7A \\sim C16-F8A \\sim C16-F9A
 with sigma of 0.1
 C1S-F1S \\sim C1S-F2S \\sim C1S-F3S
 with sigma of 0.1
 C3SA-F4SA \\sim C3SA-F5SA \\sim C3SA-F6SA
 with sigma of 0.1
 C3S-F4S \\sim C3S-F5S \\sim C3S-F6S
 with sigma of 0.1
 C14-F4 \\sim C14-F5 \\sim C14-F6 \\sim C14-F4A \\sim C14-F5A \\sim C14-F6A
 with sigma of 0.1
 C15A-C14 \\sim C15-C14 \\sim C17A-C16 \\sim C17-C16
 with sigma of 0.02
 C1SA-F1SA \\sim C1SA-F2SA \\sim C1SA-F3SA
 with sigma of 0.1
 C18-F10A \\sim C18-F11A \\sim C18-F12A \\sim C18-F10B \\sim C18-F11B \\sim
C18-F12B \\sim C18-F10 ~
 C18-F11 \\sim C18-F12
 with sigma of 0.1
 C12-F1B \\sim C12-F2B \\sim C12-F3B \\sim C12-F1 \\sim C12-F2 \\sim C12-F3
\\sim C12-F1A \\sim C12-F2A ~
 C12-F3A
 with sigma of 0.1
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 1*[Sof(F10)+Sof(F11)+Sof(F12)]+1*[Sof(F10A)+Sof(F11A)+Sof(F12A)]+1*[Sof(F10B)+
 Sof(F11B)+Sof(F12B)]=1 with esd of 0
 1*[Sof(F1)+Sof(F2)+Sof(F3)]+1*[Sof(F1A)+Sof(F2A)+Sof(F3A)]+1*[Sof(F1B)+
 Sof(F2B)+Sof(F3B)]=1 with esd of 0
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=FVAR(3)
 Sof(C15A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(4)
 Sof(C15)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(4)
 Sof(C17A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(5)
 Sof(C17)=Sof(F7)=Sof(F8)=Sof(F9)=FVAR(5)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(6)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(7)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=FVAR(8)
 Sof(O1SA)=Sof(O2SA)=Sof(H2SA)=Sof(C1SA)=Sof(C2SA)=Sof(F1SA)=Sof(F2SA)=
 Sof(F3SA)=1-FVAR(9)
 Sof(O1S)=Sof(O2S)=Sof(H2S)=Sof(C1S)=Sof(C2S)=Sof(F1S)=Sof(F2S)=Sof(F3S)=FVAR(9)
 Sof(O3SA)=Sof(O4SA)=Sof(H4SA)=Sof(C3SA)=Sof(C4SA)=Sof(F4SA)=Sof(F5SA)=
 Sof(F6SA)=1-FVAR(10)
 Sof(O3S)=Sof(O4S)=Sof(H4S)=Sof(C3S)=Sof(C4S)=Sof(F4S)=Sof(F5S)=Sof(F6S)=
 FVAR(10)
 Uiso(O3SA)=Uiso(O4SA)=Uiso(C3SA)=Uiso(C4SA)=Uiso(F4SA)=Uiso(F5SA)=Uiso(F6SA)=
 FVAR(11)
5.a Free rotating group:
 O1S(O2S,H2S,C1S,C2S), O1SA(O2SA,H2SA,C1SA,C2SA), O3S(O4S,H4S,C3S,C4S),
 O3SA(O4SA,H4SA,C3SA,C4SA)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C9(H9), C10(H10), C11(H11)
;
_shelx_res_checksum              30124
_shelx_hkl_checksum              80306
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'