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_7713418
_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), C300 H216 Ag25 Cl6 Cu4 F12 Fe6 P12, 31[CH3CH2OCH2CH3]'
_chemical_formula_sum            'C300 H216 Ag25.08 Cl6 Cu3.92 F24 Fe6 P12 Sb2'
_chemical_formula_weight         8393.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-15 deposited with the CCDC.	2023-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0344(2)
_cell_length_b                   37.8184(3)
_cell_length_c                   40.5275(4)
_cell_measurement_reflns_used    76225
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.7850
_cell_measurement_theta_min      2.3600
_cell_volume                     33442.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -14.00  67.00   0.50    0.80    --   -1.25  71.00   2.00  162
  2  \w    -65.00  11.00   0.50    0.80    --   -1.25 -71.00-128.00  152
  3  \w     27.00  52.00   0.50    2.00    --   82.87 -71.00-128.00   50
  4  \w     84.00 128.00   0.50    2.00    --   82.87  71.00   2.00   88
  5  \w   -156.00 -80.00   0.50    2.00    --  -85.37 -71.00-128.00  152
  6  \w    -65.00 -33.00   0.50    2.00    --  -85.37  71.00   2.00   64
  7  \w    -50.00  -4.00   0.50    0.80    --   -1.25   0.00-120.00   92
  8  \w    -14.00  12.00   0.50    0.80    --   -1.25 -99.00  90.00   52
  9  \w    129.00 155.00   0.50    2.00    --   82.87 125.00  30.00   52
 10  \w     20.00  50.00   0.50    2.00    --   82.87-125.00  90.00   60
 11  \w     18.00  44.00   0.50    2.00    --   82.87 -38.00  90.00   52
 12  \w     18.00  44.00   0.50    2.00    --   82.87 -38.00 150.00   52
 13  \w     18.00  99.00   0.50    2.00    --   82.87 -77.00  60.00  162
 14  \w     57.00 110.00   0.50    2.00    --   82.87-125.00-180.00  106
 15  \w     83.00 125.00   0.50    2.00    --   82.87 125.00  30.00   84
 16  \w     39.00 111.00   0.50    2.00    --   82.87-125.00 -30.00  144
 17  \w     12.00  44.00   0.50    2.00    --   82.87 -38.00 -60.00   64
 18  \w     64.00  90.00   0.50    2.00    --   82.87-125.00  90.00   52
 19  \w     18.00 105.00   0.50    2.00    --   82.87 -99.00-180.00  174
 20  \w     22.00  50.00   0.50    2.00    --   82.87-125.00-180.00   56
 21  \w     15.00  63.00   0.50    2.00    --   82.87 -57.00  60.00   96
 22  \w     37.00  87.00   0.50    2.00    --   82.87   0.00  30.00  100
 23  \w     13.00 104.00   0.50    2.00    --   82.87 -99.00-120.00  182
 24  \w     19.00 105.00   0.50    2.00    --   82.87-125.00  30.00  172
 25  \w    -41.00 -16.00   0.50    2.00    --  -85.37  38.00 150.00   50
 26  \w    -81.00 -56.00   0.50    2.00    --  -85.37  77.00  60.00   50
 27  \w    -40.00 -14.00   0.50    2.00    --  -85.37  57.00-180.00   52
 28  \w    -41.00 -16.00   0.50    2.00    --  -85.37  38.00 -90.00   50
 29  \w    -41.00 -16.00   0.50    2.00    --  -85.37  38.00-180.00   50
 30  \w    -44.00 -19.00   0.50    2.00    --  -85.37 125.00  60.00   50
 31  \w   -112.00 -77.00   0.50    2.00    --  -85.37 125.00  60.00   70
 32  \w    -83.00 -47.00   0.50    2.00    --  -85.37  77.00  30.00   72
 33  \w    -41.00 -16.00   0.50    2.00    --  -85.37  38.00 -60.00   50
 34  \w   -152.00 -76.00   0.50    2.00    --  -85.37 -57.00 -60.00  152
 35  \w    -40.00 -15.00   0.50    2.00    --  -85.37  38.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            184596
_diffrn_reflns_point_group_measured_fraction_full 0.793
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        63.998
_diffrn_reflns_theta_max         63.998
_diffrn_reflns_theta_min         2.337
_exptl_absorpt_coefficient_mu    16.451
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light red'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             16257
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.493
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.234
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.247(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2883
_refine_ls_number_reflns         44057
_refine_ls_number_restraints     2719
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0939
_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^)+(0.1387P)^2^+643.2844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2349
_refine_ls_wR_factor_ref         0.2474
_reflns_Friedel_coverage         0.586
_reflns_Friedel_fraction_full    0.587
_reflns_Friedel_fraction_max     0.587
_reflns_number_gt                36781
_reflns_number_total             44057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01461d2.cif
_cod_data_source_block           sh-dppf-red_auto
_cod_database_code               7713418
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.753(11)
 0.247(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Shared sites
{Cu1, Ag1A}
{Cu3, Ag1B}
4. Restrained distances
 C58-C82
 1.4 with sigma of 0.01
 C278-C193
 1.42 with sigma of 0.01
 C82-C206
 1.19 with sigma of 0.01
 C278-C149
 1.2 with sigma of 0.01
 F17-C184
 1.3 with sigma of 0.02
 Sb2-F19 = Sb2-F20 = Sb2-F22 = Sb2-F24
 1.88 with sigma of 0.02
 Sb2-F21 = Sb2-F23
 1.87 with sigma of 0.02
 Sb2-F19 \\sim Sb2-F20 \\sim Sb2-F21 \\sim Sb2-F22 \\sim Sb2-F23 \\sim Sb2-F24
 with sigma of 0.02
 F19-F20 \\sim F19-F21 \\sim F19-F22 \\sim F19-F23 \\sim F20-F21 \\sim F20-F23
\\sim F20-F24 \\sim F21-F22
 \\sim F21-F24 \\sim F22-F23 \\sim F22-F24 \\sim F23-F24
 with sigma of 0.04
5. Restrained planarity
 F18, C256, C257, C258, C259, C260, C261
 with sigma of 0.1
6. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Sb2 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Sb1) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F16) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C272) \\sim Ueq, Uanis(C273) \\sim Ueq, Uanis(C274) \\sim Ueq,
Uanis(C269) \\sim Ueq, Uanis(C270) \\sim Ueq, Uanis(C271) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(F1) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C173) \\sim Ueq, Uanis(C178) \\sim Ueq, Uanis(C177) \\sim Ueq,
Uanis(C176) \\sim Ueq, Uanis(C175) \\sim Ueq, Uanis(C174) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C199) \\sim Ueq, Uanis(C131) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cu1) = Uanis(Ag1A)
Uanis(Cu3) = Uanis(Ag1B)
7. Rigid body (RIGU) restrains
 Sb1, F6, F10, F12, F13, F14, F16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Sb2, F19, F20, F21, F22, F23, F24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Sof(Ag1A)=1-FVAR(1)
 Sof(Cu1)=FVAR(1)
 Sof(Ag1B)=1-FVAR(2)
 Sof(Cu3)=FVAR(2)
 Fixed Z: Ag1(0.27774)
9.a Ternary CH refined with riding coordinates:
 C63(H63), C133(H133), C162(H162), C163(H163), C191(H191), C209(H209),
 C288(H288)
9.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C40(H40), C41(H41),
  C42(H42), C43(H43), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C59(H59), C61(H61), C62(H62),
  C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72),
 C73(H73), C74(H74), C75(H75), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
  C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90),
 C92(H92), C93(H93), C94(H94), C96(H96), C97(H97), C98(H98), C99(H99),
 C100(H100), C101(H101), C102(H102), C104(H104), C105(H105), C106(H106),
 C108(H108), C109(H109), C110(H110), C111(H111), C112(H112), C113(H113),
 C114(H114), C116(H116), C117(H117), C118(H118), C119(H119), C121(H121),
 C123(H123), C124(H124), C125(H125), C126(H126), C128(H128), C129(H129),
 C130(H130), C132(H132), C135(H135), C136(H136), C138(H138), C139(H139),
 C140(H140), C141(H141), C143(H143), C144(H144), C145(H145), C146(H146),
 C148(H148), C150(H150), C152(H152), C153(H153), C154(H154), C156(H156),
 C157(H157), C158(H158), C159(H159), C161(H161), C164(H164), C166(H166),
 C167(H167), C169(H169), C171(H171), C173(H173), C174(H174), C175(H175),
 C176(H176), C177(H177), C181(H181), C182(H182), C183(H183), C185(H185),
 C189(H189), C190(H190), C192(H192), C194(H194), C196(H196), C197(H197),
 C198(H198), C202(H202), C203(H203), C204(H204), C205(H205), C208(H208),
 C210(H210), C212(H212), C215(H215), C216(H216), C217(H217), C218(H218),
 C219(H219), C220(H220), C221(H221), C222(H222), C223(H223), C224(H224),
 C226(H226), C228(H228), C229(H229), C230(H230), C232(H232), C234(H234),
 C235(H235), C236(H236), C239(H239), C240(H240), C241(H241), C242(H242),
 C243(H243), C245(H245), C246(H246), C247(H247), C248(H248), C249(H249),
 C251(H251), C253(H253), C254(H254), C255(H255), C256(H256), C258(H258),
 C259(H259), C260(H260), C262(H262), C264(H264), C265(H265), C266(H266),
 C267(H267), C269(H269), C271(H271), C272(H272), C273(H273), C274(H274),
 C285(H285), C286(H286), C287(H287), C290(H290), C291(H291), C292(H292),
 C293(H293), C294(H294), C296(H296), C297(H297), C298(H298), C299(H299),
 C300(H300)
9.c Fitted pentagon refined as free rotating group:
 C107(C108,C109,C110,C111), C113(C114,C115,C116,C117), C132(C133,C134,C135,
 C136), C137(C138,C139,C140,C141), C150(C151,C152,C153,C154), C155(C156,C157,
 C158,C159), C160(C161,C162,C163,C164), C188(C189,C190,C191,C192), C201(C202,
 C203,C204,C205), C208(C209,C210,C211,C212), C284(C285,C286,C287,C288)
9.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C8(C9,C10,C11,C12,C13), C14(C15,C16,C17,C18,C19), C20(C21,
 C22,C23,C24,C25), C26(C27,C28,C29,C30,C31), C32(C33,C34,C35,C36,C37), C38(C39,
 C40,C41,C42,C43), C45(C46,C47,C48,C49,C50), C51(C52,C53,C54,C55,C56), C57(C58,
 C59,C60,C61,C62), C64(C65,C66,C67,C68,C69), C70(C71,C72,C73,C74,C75), C76(C77,
 C78,C79,C80,C81), C83(C84,C85,C86,C87,C88), C89(C90,C91,C92,C93,C94), C95(C96,
 C97,C98,C99,C100), C101(C102,C103,C104,C105,C106), C119(C120,C121,C122,C123,
 C124), C125(C126,C127,C128,C129,C130), C143(C144,C145,C146,C147,C148),
 C166(C167,C168,C169,C170,C171), C173(C174,C175,C176,C177,C178), C181(C182,C183,
 C184,C185,C186), C193(C194,C195,C196,C197,C198), C214(C215,C216,C217,C218,
 C219), C220(C221,C222,C223,C224,C225), C226(C227,C228,C229,C230,C231),
 C232(C233,C234,C235,C236,C237), C238(C239,C240,C241,C242,C243), C244(C245,C246,
 C247,C248,C249), C250(C251,C252,C253,C254,C255), C256(C257,C258,C259,C260,
 C261), C262(C263,C264,C265,C266,C267), C269(C270,C271,C272,C273,C274),
 C289(C290,C291,C292,C293,C294), C295(C296,C297,C298,C299,C300)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              460
_shelx_fab_checksum              85183
_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
;