DppfCuBH4: new reducing agents for the synthesis of ferrocene-functionalized metal nanoclusters
Wang, Meng; Li, Simin; Chen, Hui Jun; Sun, Xueli; Sun, Jing; jia, yanyuan; Guo, Shuo; SUN, Cunfa; Shen, Hui; Dalton Transactions  (2023) –; doi:10.1039/D3DT01461D

data_7713417
_publ_section_title
;
 DppfCuBH4: new reducing agents for the synthesis of
 ferrocene-functionalized metal nanoclusters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01461D
_journal_year                    2023
_chemical_formula_moiety
'2(F6 Sb), C170 H140 Ag4 Cl2 Fe5 P10, 4.5[CH3CH2OCH2CH3]'
_chemical_formula_sum            'C188 H185 Ag4 Cl2 F12 Fe5 O4.5 P10 Sb2'
_chemical_formula_weight         4079.18
_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     dual
_audit_creation_date             2023-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-05-15 deposited with the CCDC.	2023-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                68.798(11)
_cell_angle_beta                 81.147(9)
_cell_angle_gamma                89.787(11)
_cell_formula_units_Z            1
_cell_length_a                   15.428(2)
_cell_length_b                   15.617(2)
_cell_length_c                   20.1332(17)
_cell_measurement_reflns_used    2481
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      61.1250
_cell_measurement_theta_min      4.0280
_cell_volume                     4461.5(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -15.00  19.00   1.00    1.00    --    0.00 -77.00  30.00   34
  2  \w    -83.00 -39.00   1.00    1.00    --    0.00-178.00   0.00   44
  3  \w    -12.00  21.00   1.00    1.00    --    0.00 -77.00 -60.00   33
  4  \w    -17.00  27.00   1.00    1.00    --    0.00 -77.00 -90.00   44
  5  \w    -30.00  42.00   1.00    1.00    --    0.00  77.00-120.00   72
  6  \w    -17.00  23.00   1.00    1.00    --    0.00 -77.00  60.00   40
  7  \w     22.00 109.00   1.00    2.50    --   87.81 -61.00   0.00   87
  8  \w    117.00 158.00   1.00    2.50    --   87.81  77.00-120.00   41
  9  \w    103.00 159.00   1.00    2.50    --   87.81  77.00  90.00   56
 10  \w    127.00 159.00   1.00    2.50    --   87.81  77.00 -60.00   32
 11  \w     67.00 111.00   1.00    2.50    --   87.81-125.00 -60.00   44
 12  \w     27.00  99.00   1.00    2.50    --   87.81 -45.00 150.00   72
 13  \w     82.00 111.00   1.00    2.50    --   87.81-122.00 111.00   29
 14  \w     26.00  51.00   1.00    2.50    --   87.81-122.00 111.00   25
 15  \w     32.00 100.00   1.00    2.50    --   87.81 -77.00 -60.00   68
 16  \w     13.00  98.00   1.00    2.50    --   87.81 -94.00 150.00   85
 17  \w     67.00 100.00   1.00    2.50    --   87.81  45.00 -60.00   33
 18  \w    124.00 150.00   1.00    2.50    --   87.81  45.00 -60.00   26
 19  \w     48.00 164.00   1.00    2.50    --   87.81  15.00  60.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0089801000
_diffrn_orient_matrix_UB_12      0.0804898000
_diffrn_orient_matrix_UB_13      -0.0732903000
_diffrn_orient_matrix_UB_21      0.0000847000
_diffrn_orient_matrix_UB_22      0.0689292000
_diffrn_orient_matrix_UB_23      0.0387107000
_diffrn_orient_matrix_UB_31      0.1008216000
_diffrn_orient_matrix_UB_32      -0.0012275000
_diffrn_orient_matrix_UB_33      -0.0071716000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1580
_diffrn_reflns_av_unetI/netI     0.2762
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25864
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             2061
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.853
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         14131
_refine_ls_number_restraints     935
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.2354
_refine_ls_R_factor_gt           0.0984
_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^)+(0.0674P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3878
_reflns_number_total             14131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01461d2.cif
_cod_data_source_block           20211210-c6-yellow_auto
_cod_original_formula_sum        'C188 H185 Ag4 Cl2 F12 Fe5 O4.50 P10 Sb2'
_cod_database_code               7713417
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P5-C92
 1.8 with sigma of 0.01
 Sb1B-F10
 1.8 with sigma of 0.02
 C86-P6
 1.8 with sigma of 0.01
 Sb1B-F9
 1.8 with sigma of 0.02
 Sb1B-F12
 1.8 with sigma of 0.02
 Sb1B-F7
 1.8 with sigma of 0.02
 F11-Sb1B
 1.9 with sigma of 0.02
 Sb1B-F8
 1.9 with sigma of 0.02
 Sb1-F1
 1.8 with sigma of 0.02
 P6-C71
 1.8 with sigma of 0.02
 P5-C71
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Sb1B \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Sb1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
P5 \\sim P6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C7 \\sim C11 \\sim C20 \\sim C28 \\sim C56 \\sim C63: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(F11) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(Sb1B) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F6) \\sim Ueq, Uanis(Sb1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(C88) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C91)
\\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C95) \\sim Ueq,
Uanis(C94) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C97)
\\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(P6) \\sim Ueq, Uanis(P5) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C80, C81, C82, C83, C84, C85
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C74, C75, C76, C77, C78, C79
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C5, C14, C29, C34, C35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C9, C16, C19, C30, C40, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C86, C87, C88, C89, C90, C91, C92, C93, C94, C95, C96, C97
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C68, C69, C70, C71, C72
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C24, C33, C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6, C15, C17, C18, C25, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C22, C23, C46, C50, C59
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C10, C26, C36, C64, C66
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C12, C31, C48, C60, C65
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C27, C52, C57, C62, C67, C73
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Sb1, F1, F2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Sb1B, F7, F8, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(P5)=Sof(C74)=Sof(H74)=Sof(C75)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=
 Sof(C78)=Sof(H78)=Sof(C79)=Sof(H79)=Sof(C92)=Sof(C93)=Sof(H93)=Sof(C94)=
 Sof(H94)=Sof(C95)=Sof(H95)=Sof(C96)=Sof(H96)=Sof(C97)=Sof(H97)=1-FVAR(1)
 Sof(P6)=Sof(C80)=Sof(H80)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(H82)=Sof(C83)=
 Sof(C84)=Sof(H84)=Sof(C85)=Sof(H85)=Sof(C86)=Sof(C87)=Sof(H87)=Sof(C88)=
 Sof(H88)=Sof(C89)=Sof(H89)=Sof(C90)=Sof(H90)=Sof(C91)=Sof(H91)=FVAR(1)
 Sof(Sb1B)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(2)
 Sof(Sb1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C10(H10), C66(H66)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
  C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C65(H65), C67(H67), C68(H68), C69(H69),
 C70(H70), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77), C78(H78), C79(H79),
  C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C87(H87), C88(H88),
 C89(H89), C90(H90), C91(H91), C93(H93), C94(H94), C95(H95), C96(H96), C97(H97)
6.c Fitted pentagon refined as free rotating group:
 C41(C42,C43,C44,C45), C68(C69,C70,C71,C72)
6.d Fitted hexagon refined as free rotating group:
 C74(C75,C76,C77,C78,C79), C80(C81,C82,C83,C84,C85), C86(C87,C88,C89,C90,C91),
 C92(C93,C94,C95,C96,C97)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75619
_shelx_fab_checksum              85462
_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 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.616