Bimolecular fusion of [Pd<sub>3</sub>(μ-CN-C<sub>6</sub>H<sub>3</sub>Me<sub>2</sub>-2,6)<sub>3</sub>(CN-C<sub>6</sub>H<sub>3</sub>Me<sub>2</sub>-2,6)<sub>3</sub>] induced by Ph<sub>2</sub>GeH<sub>2</sub>: formation of the redox-active Pd<sub>6</sub>Ge<sub>2</sub> complex.
Koizumi, Take-Aki; Tanaka, Kimiya; Tsuchido, Yoshitaka; Tanabe, Makoto; Ide, Tomohito; Osakada, Kohtaro; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7541–7545; doi:10.1039/c9dt00814d

data_7049856
_publ_section_title
;
 Bimolecular fusion of
 [Pd<sub>3</sub>(\m-CN-C<sub>6</sub>H<sub>3</sub>Me<sub>2</sub>-2,6)<sub>3</sub>(CN-C<sub>6</sub>H<sub>3</sub>Me<sub>2</sub>-2,6)<sub>3</sub>]
 induced by Ph<sub>2</sub>GeH<sub>2</sub>: formation of the redox-active
 Pd<sub>6</sub>Ge<sub>2</sub> complex.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7541
_journal_page_last               7545
_journal_paper_doi               10.1039/c9dt00814d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C114 H110 Ge2 N10 Pd6, 0.5(C4 H8 O), 0.5(C6 H13.17)'
_chemical_formula_sum            'C119 H119.99 Ge2 N10 O0.5 Pd6'
_chemical_formula_weight         2481.81
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-04 deposited with the CCDC.    2019-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                83.0180(10)
_cell_angle_beta                 74.7000(10)
_cell_angle_gamma                62.5470(10)
_cell_formula_units_Z            2
_cell_length_a                   15.27410(10)
_cell_length_b                   16.00210(10)
_cell_length_c                   26.7383(3)
_cell_measurement_reflns_used    58188
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.8800
_cell_measurement_theta_min      3.4020
_cell_volume                     5593.82(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     21.00  54.00   0.50    0.05    --   42.05  57.00 -60.00   66
  2  \w     83.00 109.00   0.50    0.05    --   42.05  57.00 -60.00   52
  3  \w     99.00 155.00   0.50    0.11    --  106.13 142.00  64.00  112
  4  \w     87.00 123.00   0.50    0.11    --  106.13  45.00   0.00   72
  5  \w    128.00 154.00   0.50    0.11    --  106.13  45.00   0.00   52
  6  \w    111.00 173.00   0.50    0.11    --  106.13  15.00  60.00  124
  7  \w    120.00 173.00   0.50    0.11    --  106.13  15.00 120.00  106
  8  \w     78.00 164.00   0.50    0.11    --  106.13  77.00 150.00  172
  9  \w     88.00 143.00   0.50    0.11    --  106.13  61.00 -30.00  110
 10  \w    120.00 146.00   0.50    0.11    --  106.13 127.00-105.00   52
 11  \w    102.00 128.00   0.50    0.11    --  106.13  61.00-150.00   52
 12  \w     88.00 173.00   0.50    0.11    --  106.13  45.00 -90.00  170
 13  \w     83.00 169.00   0.50    0.11    --  106.13  61.00-120.00  172
 14  \w     78.00 104.00   0.50    0.11    --  106.13  15.00  60.00   52
 15  \w     72.00  98.00   0.50    0.11    --  106.13  15.00 120.00   52
 16  \w     41.00  73.00   0.50    0.11    --  106.13 -61.00  30.00   64
 17  \w     82.00 107.00   0.50    0.11    --  106.13 -77.00  30.00   50
 18  \w     73.00 101.00   0.50    0.11    --  106.13 -94.00  30.00   56
 19  \w     96.00 125.00   0.50    0.11    --  106.13-142.00   8.00   58
 20  \w     64.00 106.00   0.50    0.11    --  106.13-125.00 -60.00   84
 21  \w     50.00 103.00   0.50    0.05    --   42.05-142.00   8.00  106
 22  \w     33.00  72.00   0.50    0.11    --  106.13 -61.00 -90.00   78
 23  \w     46.00  71.00   0.50    0.11    --  106.13 -61.00 -30.00   50
 24  \w     43.00  68.00   0.50    0.11    --  106.13 -94.00  30.00   50
 25  \w     40.00 105.00   0.50    0.11    --  106.13 -94.00 -30.00  130
 26  \w     35.00  67.00   0.50    0.11    --  106.13 -61.00-120.00   64
 27  \w     33.00 106.00   0.50    0.11    --  106.13 -94.00-150.00  146
 28  \w     40.00  69.00   0.50    0.11    --  106.13 -61.00-180.00   58
 29  \w     33.00 111.00   0.50    0.11    --  106.13-125.00-150.00  156
 30  \w     35.00  76.00   0.50    0.11    --  106.13 -77.00  30.00   82
 31  \w     35.00  65.00   0.50    0.11    --  106.13 -61.00  60.00   60
 32  \w     32.00  61.00   0.50    0.11    --  106.13 -61.00 120.00   58
 33  \w     73.00 114.00   0.50    0.11    --  106.13-127.00 178.00   82
 34  \w     34.00  87.00   0.50    0.05    --   42.05-127.00 178.00  106
 35  \w     34.00 100.00   0.50    0.11    --  106.13-125.00 150.00  132
 36  \w     53.00 112.00   0.50    0.05    --   42.05  57.00 150.00  118
 37  \w     21.00  47.00   0.50    0.05    --   42.05  57.00 150.00   52
 38  \w    -36.00  26.00   0.50    0.05    --   42.05 -19.00   0.00  124
 39  \w    -37.00  28.00   0.50    0.05    --   42.05 -19.00 -90.00  130
 40  \w    -37.00  27.00   0.50    0.05    --   42.05 -19.00-150.00  128
 41  \w     90.00 163.00   0.50    0.11    --  106.13  61.00-180.00  146
 42  \w    -37.00  28.00   0.50    0.05    --   42.05 -19.00 150.00  130
 43  \w    -69.00 -15.00   0.50    0.05    --  -19.00 125.00  30.00  108
 44  \w    -71.00 -46.00   0.50    0.05    --  -19.00 142.00  64.00   50
 45  \w    -68.00 -43.00   0.50    0.05    --  -19.00 127.00-105.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0150733000
_diffrn_orient_matrix_UB_12      -0.0315232000
_diffrn_orient_matrix_UB_13      -0.0479763000
_diffrn_orient_matrix_UB_21      0.0575078000
_diffrn_orient_matrix_UB_22      0.0511249000
_diffrn_orient_matrix_UB_23      -0.0354307000
_diffrn_orient_matrix_UB_31      0.1007277000
_diffrn_orient_matrix_UB_32      -0.0903467000
_diffrn_orient_matrix_UB_33      -0.0033169000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            69463
_diffrn_reflns_point_group_measured_fraction_full 0.737
_diffrn_reflns_point_group_measured_fraction_max 0.709
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.023
_diffrn_reflns_theta_min         3.389
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.589
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       prism
_exptl_crystal_F_000             2496
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, Hexane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 9429 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.025(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2538
_refine_ls_number_reflns         32657
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.455
_reflns_Friedel_fraction_full    0.478
_reflns_Friedel_fraction_max     0.443
_reflns_number_gt                31601
_reflns_number_total             32657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00814d2.cif
_cod_data_source_block           koz528
_cod_depositor_comments          'Adding full bibliography for 7049856.cif.'
_cod_original_formula_sum        'C119 H119.99 Ge2 N10 O0.50 Pd6'
_cod_database_code               7049856
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C114H110Ge2N10Pd6
_diffrn_oxdiff_digest_frames
;
01a032333c6a0958feff4cec4cd8607be804122e479
;
_diffrn_oxdiff_digest_hkl
;
01c6cfc7023f5fe78af814c32b4a823615f860
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H23O,H23P,H235} of C235, {H23A,H23B,H236} of C236, All
  C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups, {H10A,H10B,H10C} of C104, {H20A,H20B,H20C} of
  C209, {H10D,H10E,H10F} of C105, {H42A,H42B,H42C} of C42, {H20D,H20E,H20F} of
  C200, {H18A,H18B,H18C} of C183, {H11A,H11B,H11C} of C114, {H60A,H60B,H60C} of
  C60, {H19A,H19B,H19C} of C191, {H18D,H18E,H18F} of C182, {H19D,H19E,H19F} of
  C192, {H21G,H21H,H21I} of C219, {H15D,H15E,H15F} of C155, {H15A,H15B,H15C} of
  C156, {H32A,H32B,H32C} of C32, {H17A,H17B,H17C} of C173, {H68A,H68B,H68C} of
  C68, {H95A,H95B,H95C} of C95, {H50A,H50B,H50C} of C50, {H87A,H87B,H87C} of
  C87, {H17D,H17E,H17F} of C174, {H14A,H14B,H14C} of C147, {H77A,H77B,H77C} of
  C77, {H20G,H20H,H20I} of C201, {H41A,H41B,H41C} of C41, {H14D,H14E,H14F} of
  C146, {H59A,H59B,H59C} of C59, {H22D,H22E,H22F} of C227, {H21D,H21E,H21F} of
  C218, {H96A,H96B,H96C} of C96, {H51A,H51B,H51C} of C51, {H11D,H11E,H11F} of
  C113, {H86A,H86B,H86C} of C86, {H21A,H21B,H21C} of C210, {H16A,H16B,H16C} of
  C164, {H22A,H22B,H22C} of C228, {H78A,H78B,H78C} of C78, {H33A,H33B,H33C} of
  C33, {H16D,H16E,H16F} of C165, {H69A,H69B,H69C} of C69
2. Others
 Sof(H236)=Sof(H23F)=Sof(H23G)=Sof(H23H)=Sof(C237)=Sof(H23S)=Sof(H23T)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(H23D)=Sof(H23E)=Sof(C240)=Sof(H24A)=
 Sof(H24B)=FVAR(1)
 Sof(H23L)=Sof(H23M)=Sof(H23N)=Sof(H235)=Sof(C234)=Sof(H23U)=Sof(H23V)=1-FVAR(2)
 Sof(H23I)=Sof(H23J)=Sof(H23K)=Sof(H23O)=Sof(H23P)=Sof(C239)=Sof(H23Q)=
 Sof(H23R)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C229(H22G,H22H), C230(H23W,H23X), C231(H23Y,H), C232(H23Z,HA), C236(H23A,
 H23B), C235(H23O,H23P), C239(H23Q,H23R), C240(H24A,H24B), C237(H23S,H23T),
 C234(H23U,H23V)
3.b Aromatic/amide H refined with riding coordinates:
 C138(H138), C47(H47), C46(H46), C137(H137), C120(H120), C134(H134), C20(H20),
 C126(H126), C136(H136), C18(H18), C84(H84), C91(H91), C57(H57), C100(H100),
 C128(H128), C198(H198), C82(H82), C178(H178), C196(H196), C130(H130), C15(H15),
  C206(H206), C169(H169), C117(H117), C11(H11), C21(H21), C170(H170), C5(H5),
 C122(H122), C205(H205), C189(H189), C118(H118), C83(H83), C14(H14), C39(H39),
 C38(H38), C12(H12), C162(H162), C123(H123), C125(H125), C6(H6), C160(H160),
 C92(H92), C2(H2), C179(H179), C48(H48), C152(H152), C24(H24), C153(H153),
 C8(H8), C197(H197), C30(H30), C22(H22), C151(H151), C23(H23), C3(H3),
 C116(H116), C101(H101), C132(H132), C124(H124), C75(H75), C171(H171), C66(H66),
  C188(H188), C161(H161), C73(H73), C207(H207), C119(H119), C37(H37), C17(H17),
 C109(H109), C180(H180), C102(H102), C93(H93), C10(H10), C29(H29), C187(H187),
 C9(H9), C74(H74), C144(H144), C111(H111), C56(H56), C225(H225), C110(H110),
 C131(H131), C143(H143), C129(H129), C28(H28), C142(H142), C65(H65), C135(H135),
  C64(H64), C223(H223), C214(H214), C215(H215), C16(H16), C224(H224), C55(H55),
 C216(H216), C4(H4), C236(H236), C235(H235)
3.c Idealised Me refined as rotating group:
 C104(H10A,H10B,H10C), C209(H20A,H20B,H20C), C105(H10D,H10E,H10F), C42(H42A,
 H42B,H42C), C200(H20D,H20E,H20F), C183(H18A,H18B,H18C), C114(H11A,H11B,H11C),
 C60(H60A,H60B,H60C), C191(H19A,H19B,H19C), C182(H18D,H18E,H18F), C192(H19D,
 H19E,H19F), C51(H51A,H51B,H51C), C96(H96A,H96B,H96C), C113(H11D,H11E,H11F),
 C86(H86A,H86B,H86C), C210(H21A,H21B,H21C), C164(H16A,H16B,H16C), C228(H22A,
 H22B,H22C), C78(H78A,H78B,H78C), C33(H33A,H33B,H33C), C165(H16D,H16E,H16F),
 C69(H69A,H69B,H69C), C218(H21D,H21E,H21F), C173(H17A,H17B,H17C), C68(H68A,H68B,
 H68C), C95(H95A,H95B,H95C), C50(H50A,H50B,H50C), C87(H87A,H87B,H87C),
 C174(H17D,H17E,H17F), C147(H14A,H14B,H14C), C77(H77A,H77B,H77C), C201(H20G,
 H20H,H20I), C41(H41A,H41B,H41C), C146(H14D,H14E,H14F), C59(H59A,H59B,H59C),
 C227(H22D,H22E,H22F), C32(H32A,H32B,H32C), C219(H21G,H21H,H21I), C238(H23C,
 H23D,H23E), C238(H23F,H23G,H23H), C233(H23I,H23J,H23K), C233(H23L,H23M,H23N),
 C156(H15A,H15B,H15C), C155(H15D,H15E,H15F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.835