Synthesis of an expanded pincer ligand and its bimetallic coinage metal complexes.
Delaney, Andie R.; Yu, Li-Juan; Coote, Michelle L.; Colebatch, Annie L.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11909–11917; doi:10.1039/d1dt01741a

data_7707976
_publ_section_title
;
 Synthesis of an expanded pincer ligand and its bimetallic coinage metal
 complexes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11909
_journal_page_last               11917
_journal_paper_doi               10.1039/d1dt01741a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C48 H80 Ag2 N4 O4 P4, 2(C32 H12 B F24)'
_chemical_formula_sum            'C112 H104 Ag2 B2 F48 N4 O4 P4'
_chemical_formula_weight         2843.23
_chemical_name_systematic        tBuPONNOP2Ag2BArF42
_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             2021-05-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                74.616(6)
_cell_angle_beta                 70.234(6)
_cell_angle_gamma                66.202(6)
_cell_formula_units_Z            2
_cell_length_a                   16.8129(10)
_cell_length_b                   20.1783(13)
_cell_length_c                   21.3753(14)
_cell_measurement_reflns_used    9660
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      70.1760
_cell_measurement_theta_min      4.4470
_cell_volume                     6173.9(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.949
_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    -85.00  -9.00   1.00    4.57    --  -35.53 125.00  30.00   76
  2  \w    -65.00  36.00   1.00    4.57    --  -35.53  19.00  60.00  101
  3  \w    -96.00  -6.00   1.00    4.57    --  -35.53 -19.00-150.00   90
  4  \w    -83.00 -30.00   1.00    4.57    --  -35.53 125.00-180.00   53
  5  \w     22.00  68.00   1.00    4.57    --   35.53 -99.00   0.00   46
  6  \w     19.00 100.00   1.00    4.57    --   35.53  57.00-180.00   81
  7  \w     41.00 117.00   1.00   18.28    --  105.15 -45.00  90.00   76
  8  \w     52.00 109.00   1.00   18.28    --  105.15-111.00-120.00   57
  9  \w    103.00 173.00   1.00   18.28    --  105.15  77.00 150.00   70
 10  \w     39.00 119.00   1.00   18.28    --  105.15 -45.00   0.00   80
 11  \w    108.00 145.00   1.00   18.28    --  105.15  77.00 -60.00   37
 12  \w     50.00 106.00   1.00   18.28    --  105.15 -95.00 -90.00   56
 13  \w    141.00 170.00   1.00   18.28    --  105.15  77.00   0.00   29
 14  \w     37.00 109.00   1.00   18.28    --  105.15-111.00 150.00   72
 15  \w     36.00 106.00   1.00   18.28    --  105.15 -95.00   0.00   70
 16  \w     37.00 123.00   1.00   18.28    --  105.15 -45.00-150.00   86
 17  \w     46.00 164.00   1.00   18.28    --  105.15   0.00 -60.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0879557000
_diffrn_orient_matrix_UB_12      -0.0532274000
_diffrn_orient_matrix_UB_13      0.0180432000
_diffrn_orient_matrix_UB_21      -0.0351792000
_diffrn_orient_matrix_UB_22      0.0255950000
_diffrn_orient_matrix_UB_23      0.0692291000
_diffrn_orient_matrix_UB_31      -0.0423599000
_diffrn_orient_matrix_UB_32      -0.0602807000
_diffrn_orient_matrix_UB_33      0.0296857000
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34050
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.446
_diffrn_reflns_theta_min         3.523
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.145
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light colourless'
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.932
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1889
_refine_ls_number_reflns         22812
_refine_ls_number_restraints     943
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+5.3402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16564
_reflns_number_total             22812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01741a2.cif
_cod_data_source_block           Ag2tBuPONNOP2BArF42
_cod_depositor_comments
'Adding full bibliography for 7707971--7707976.cif.'
_cod_database_code               7707976
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C112H104B2F48N4O4P4Ag2
_reflns_odcompleteness_completeness 98.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Restrained distances
 F049-C64 \\sim F0-C64
 with sigma of 0.02
 C64-F04O \\sim C64-F04P
 with sigma of 0.02
 C64-F04S \\sim C64-F04T
 with sigma of 0.02
 F049-F04O \\sim F049-F04S \\sim F04O-F04S \\sim F04T-F04P \\sim F04T-F0 \\sim
F04P-F0
 with sigma of 0.04
 C64-F049 \\sim C64-F04O \\sim C64-F04S \\sim C64-F04T \\sim C64-F04P \\sim
C64-F0 \\sim C64-C61
 with sigma of 0.02
 F011-C40 \\sim F16-C40
 with sigma of 0.02
 F01Q-C40 \\sim F01R-C40
 with sigma of 0.02
 F00P-C40 \\sim F17-C40
 with sigma of 0.02
 F01Q-F00P \\sim F01Q-F011 \\sim F16-F01R \\sim F16-F17 \\sim F00P-F011
 with sigma of 0.04
 C40-F01Q \\sim C40-F16 \\sim C40-F01R \\sim C40-F17 \\sim C40-C37 \\sim
C40-F00P \\sim C40-F011
 with sigma of 0.02
 F014-C88 \\sim F18-C88
 with sigma of 0.02
 C88-F03M \\sim C88-F03N
 with sigma of 0.02
 F026-C88 \\sim F19-C88
 with sigma of 0.02
 C88-F014 \\sim C88-F026 \\sim C88-C85 \\sim C88-F03M \\sim C88-F18 \\sim
C88-F03N \\sim C88-F19
 with sigma of 0.02
 F014-F026 \\sim F014-F03M \\sim F026-F03M \\sim F18-F03N \\sim F18-F19 \\sim
F03N-F19
 with sigma of 0.04
 F9-C39 \\sim F21-C39
 with sigma of 0.02
 F8-C39 \\sim F7-C39
 with sigma of 0.02
 F00H-C39 \\sim F20-C39
 with sigma of 0.02
 F8-F00H \\sim F8-F9 \\sim F7-F21 \\sim F7-F20 \\sim F21-F20 \\sim F00H-F9
 with sigma of 0.04
 C39-C35 \\sim C39-F8 \\sim C39-F7 \\sim C39-F21 \\sim C39-F20 \\sim C39-F00H
\\sim C39-F9
 with sigma of 0.02
 F02X-C71 \\sim F02Y-C71
 with sigma of 0.02
 F01E-C71 \\sim F01F-C71
 with sigma of 0.02
 F017-C71 \\sim F22-C71
 with sigma of 0.02
 C71-F017 \\sim C71-C67 \\sim C71-F01E \\sim C71-F02X \\sim C71-F22 \\sim
C71-F01F \\sim C71-F02Y
 with sigma of 0.02
 F017-F01E \\sim F017-F02X \\sim F01E-F02X \\sim F22-F01F \\sim F22-F02Y \\sim
F01F-F02Y
 with sigma of 0.04
 F00Z-C80 \\sim F00{-C80
 with sigma of 0.02
 F01W-C80 \\sim F01X-C80
 with sigma of 0.02
 F013-C80 \\sim F23-C80
 with sigma of 0.02
 C80-F00Z \\sim C80-F013 \\sim C80-F01X \\sim C80-F23 \\sim C80-F00{ \\sim
C80-C77 \\sim C80-F01W
 with sigma of 0.02
 F00Z-F013 \\sim F00Z-F01W \\sim F013-F01W \\sim F01X-F23 \\sim F01X-F00{ \\sim
F23-F00{
 with sigma of 0.04
 F028-C48 \\sim F12-C48
 with sigma of 0.02
 F033-C48 \\sim F11-C48
 with sigma of 0.02
 F025-C48 \\sim F10-C48
 with sigma of 0.02
 F028-F033 \\sim F028-F025 \\sim F033-F025 \\sim F10-F11 \\sim F10-F12 \\sim
F11-F12
 with sigma of 0.04
 C48-F028 \\sim C48-C45 \\sim C48-F033 \\sim C48-F025 \\sim C48-F10 \\sim
C48-F11 \\sim C48-F12
 with sigma of 0.02
 F02H-C72 \\sim F02I-C72
 with sigma of 0.02
 F04U-C72 \\sim F04V-C72
 with sigma of 0.02
 F045-C72 \\sim F13-C72
 with sigma of 0.02
 F02H-F045 \\sim F02H-F04U \\sim F045-F04U \\sim F13-F04V \\sim F13-F02I \\sim
F04V-F02I
 with sigma of 0.04
 C72-C69 \\sim C72-F02H \\sim C72-F045 \\sim C72-F04U \\sim C72-F13 \\sim
C72-F04V \\sim C72-F02I
 with sigma of 0.02
 F02N-C79 \\sim F02O-C79
 with sigma of 0.02
 F019-C79 \\sim F14-C79
 with sigma of 0.02
 F03G-C79 \\sim F03H-C79
 with sigma of 0.02
 F019-F03G \\sim F019-F02N \\sim F03G-F02N \\sim F02O-F14 \\sim F02O-F03H \\sim
F14-F03H
 with sigma of 0.04
 C79-F019 \\sim C79-F03G \\sim C79-F02N \\sim C79-C75 \\sim C79-F02O \\sim
C79-F14 \\sim C79-F03H
 with sigma of 0.02
 F04Q-C47 \\sim F04R-C47
 with sigma of 0.02
 F030-C47 \\sim F15-C47
 with sigma of 0.02
 F04I-C47 \\sim F04J-C47
 with sigma of 0.02
 C47-C43 \\sim C47-F030 \\sim C47-F04I \\sim C47-F04Q \\sim C47-F04J \\sim
C47-F15 \\sim C47-F04R
 with sigma of 0.02
 F030-F04I \\sim F030-F04Q \\sim F04I-F04Q \\sim F04J-F15 \\sim F04J-F04R \\sim
F15-F04R
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uanis(F04O) \\sim Ueq, Uanis(F04S) \\sim Ueq, Uanis(F049) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 F04T, F23, F02O, F04P, F12, F0, F15, F16, F10, F01R, F04V, F17, F03H, F18,
 F01X, F03N, F00{, F19, F11, F7, F13, F21, F02I, F20, F14, F22, F04J, F01F,
 F04R, F02Y, C88, C85, C79, C75, C80, C77, C64, C61, C71, C67, C72, C69, C39,
 C35, C47, C43, C48, C45, C40, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F00H, F02H, F049, F00P, F033, F9, F04S, F00Z, F02X, F011, F03M, F013, F04O,
 F014, F028, F017, F02N, F8, F030, F019, F03G, F01E, F045, F01Q, F04I, F01W,
 F04Q, F025, F04U, F026, C71, C67, C72, C69, C88, C85, C80, C77, C79, C75, C64,
 C61, C47, C43, C48, C45, C40, C37, C39, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F04O, F049, F04S, C64, C61
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(F04T)=Sof(F04P)=Sof(F0)=1-FVAR(1)
 Sof(F049)=Sof(F04O)=Sof(F04S)=FVAR(1)
 Sof(F16)=Sof(F01R)=Sof(F17)=1-FVAR(2)
 Sof(F00P)=Sof(F011)=Sof(F01Q)=FVAR(2)
 Sof(F18)=Sof(F03N)=Sof(F19)=1-FVAR(3)
 Sof(F014)=Sof(F026)=Sof(F03M)=FVAR(3)
 Sof(F7)=Sof(F21)=Sof(F20)=1-FVAR(4)
 Sof(F00H)=Sof(F9)=Sof(F8)=FVAR(4)
 Sof(F22)=Sof(F01F)=Sof(F02Y)=1-FVAR(5)
 Sof(F017)=Sof(F01E)=Sof(F02X)=FVAR(5)
 Sof(F01X)=Sof(F23)=Sof(F00{)=1-FVAR(6)
 Sof(F00Z)=Sof(F013)=Sof(F01W)=FVAR(6)
 Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(7)
 Sof(F025)=Sof(F028)=Sof(F033)=FVAR(7)
 Sof(F13)=Sof(F04V)=Sof(F02I)=1-FVAR(8)
 Sof(F02H)=Sof(F045)=Sof(F04U)=FVAR(8)
 Sof(F02O)=Sof(F14)=Sof(F03H)=1-FVAR(9)
 Sof(F019)=Sof(F02N)=Sof(F03G)=FVAR(9)
 Sof(F04J)=Sof(F15)=Sof(F04R)=1-FVAR(10)
 Sof(F030)=Sof(F04I)=Sof(F04Q)=FVAR(10)
5.a Aromatic/amide H refined with riding coordinates:
 C82(H016), C26(H01D), C24(H01H), C5(H01N), C3(H01S), C28(H01U), C78(H01V),
 C3B(H01Z), C54(H020), C6(H021), C58(H023), C66(H024), C5B(H027), C4(H02A),
 C46(H02E), C84(H02F), C34(H02G), C44(H02I), C4B(H02J), C6B(H02K), C50(H02L),
 C86(H02M), C60(H02O), C68(H02Q), C36(H02V), C70(H031), C76(H034), C62(H036),
 C74(H037), C42(H039), C38(H03V), C52(H03W)
5.b Idealised Me refined as rotating group:
 C13(H02B,H02C,H02D), C15(H03A,H03B,H03C), C18(H03D,H03E,H03F), C17(H03G,H03H,
 H03I), C14B(H03J,H03K,H03L), C14(H03M,H03N,H03O), C20(H03P,H03Q,H03R),
 C16(H03S,H03T,H03U), C23(H04A,H04B,H04C), C22(H04D,H04E,H04F), C15B(H04G,H04H,
 H04I), C18B(H04J,H04K,H04L), C22B(H04M,H04N,H04O), C16B(H04P,H04Q,H04R),
 C23B(H04S,H04T,H04U), C1(H04V,H04W,H04X), C19(H04Y,H,HA), C19B(H04Z,HB,HC),
 C17B(H04,HD,HE), C13B(H1,HF,HG), C24B(H2,HH,HI), C21(H3,HJ,HK), C20B(H4,HL,HM),
  C21B(H5,HN,HO)
;
_shelx_res_checksum              70682
_shelx_hkl_checksum              65319
_ins_header
;
TITL AD219_scale_2 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  16.812896  20.178277  21.375307  74.6161  70.2336  66.2021
ZERR    2.00   0.001039   0.001348   0.001439   0.0058   0.0059   0.0061
LATT  1
SFAC C H B N O F P Ag
UNIT 224.00 208.00 4.00 8.00 8.00 96.00 8.00 4.00
TREF
HKLF 4
END
;
_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 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.770