Lipshutz-type bis(amido)argentates for directed ortho argentation
Tezuka, Noriyuki; Hirano, Keiichi; Peel, Andrew J.; Wheatley, Andrew E. H.; Miyamoto, Kazunori; Uchiyama, Masanobu; Chemical Science 11 (2020) 1855–1861; doi:10.1039/C9SC06060J

data_1557459
_publ_section_title
;
 Lipshutz-type bis(amido)argentates for directed ortho argentation
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              1855
_journal_page_last               1861
_journal_paper_doi               10.1039/C9SC06060J
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C44 H72 Ag2 Li2 N4 O2, 2(C6 H6)'
_chemical_formula_sum            'C56 H84 Ag2 Li2 N4 O2'
_chemical_formula_weight         1076.90
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-18
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-10-18 deposited with the CCDC.	2020-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.316(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3743(2)
_cell_length_b                   18.2477(2)
_cell_length_c                   22.9463(3)
_cell_measurement_reflns_used    16970
_cell_measurement_temperature    93
_cell_measurement_theta_max      75.9880
_cell_measurement_theta_min      3.3680
_cell_volume                     5449.49(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -63.00 -38.00   0.50    0.80    --  -39.82   4.00 -81.00   50
  2  \w    -64.00  -3.00   0.50    2.72    --  -84.50  30.00   0.00  122
  3  \w    -64.00 -39.00   0.50    0.80    --  -39.82  -4.00 101.00   50
  4  \w    -13.00  13.00   0.50    0.80    --   39.82  -4.00 101.00   52
  5  \w     79.00 104.00   0.50    2.72    --  113.69  -4.00 101.00   50
  6  \w     50.00  79.00   0.50    2.72    --  113.69 -45.00  30.00   58
  7  \w     59.00 108.00   0.50    2.72    --  113.69 -94.00  30.00   98
  8  \w     88.00 117.00   0.50    2.72    --  113.69-125.00   0.00   58
  9  \w     76.00 117.00   0.50    2.72    --  113.69-125.00  60.00   82
 10  \w     37.00 126.00   0.50    0.80    --   39.82-178.00 150.00  178
 11  \w     34.00 102.00   0.50    2.72    --  113.69 -94.00 120.00  136
 12  \w     36.00  71.00   0.50    2.72    --  113.69-125.00   0.00   70
 13  \w     37.00  63.00   0.50    2.72    --  113.69-125.00  60.00   52
 14  \w     42.00  94.00   0.50    2.72    --  113.69 -94.00  90.00  104
 15  \w     39.00  77.00   0.50    2.72    --  113.69 -45.00 120.00   76
 16  \w     31.00  68.00   0.50    2.72    --  113.69 -30.00  90.00   74
 17  \w     32.00  69.00   0.50    2.72    --  113.69 -30.00   0.00   74
 18  \w     45.00  79.00   0.50    2.72    --  113.69 -45.00 -60.00   68
 19  \w     36.00  70.00   0.50    2.72    --  113.69 -45.00 -30.00   68
 20  \w     34.00 178.00   0.50    2.72    --  113.69   4.00 -81.00  288
 21  \w     92.00 125.00   0.50    0.80    --   39.82   4.00 -81.00   66
 22  \w     36.00  79.00   0.50    2.72    --  113.69 -45.00   0.00   86
 23  \w      3.00  90.00   0.50    0.80    --   39.82   4.00 -81.00  174
 24  \w     40.00 120.00   0.50    0.80    --   39.82 178.00 -60.00  160
 25  \w    -98.00 -72.00   0.50    0.80    --  -39.82   4.00 -81.00   52
 26  \w   -108.00 -83.00   0.50    2.72    --  -84.50   4.00 -81.00   50
 27  \w   -170.00  -1.00   0.50    2.72    --  -84.50  -4.00 101.00  338
 28  \w   -113.00 -33.00   0.50    2.72    --  -84.50  61.00  90.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0902358000
_diffrn_orient_matrix_UB_12      0.0071937000
_diffrn_orient_matrix_UB_13      -0.0308937000
_diffrn_orient_matrix_UB_21      -0.0761175000
_diffrn_orient_matrix_UB_22      -0.0004117000
_diffrn_orient_matrix_UB_23      -0.0616588000
_diffrn_orient_matrix_UB_31      -0.0080715000
_diffrn_orient_matrix_UB_32      0.0841469000
_diffrn_orient_matrix_UB_33      0.0023577000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37918
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         3.128
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              PhotonJet-S
_exptl_absorpt_coefficient_mu    6.078
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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            'clear brownish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       prism
_exptl_crystal_F_000             2264
_exptl_crystal_preparation       '4C in benzene'
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         9918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0423P)^2^+6.6478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9060
_reflns_number_total             9918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06060j2.cif
_cod_data_source_block           exp_334
_cod_depositor_comments
'Adding full bibliography for 1557456--1557459.cif.'
_cod_database_code               1557459
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C23 H36 Ag N3 O1 Li2 '
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00D(H00D), C00O(H00O), C00P(H00P), C00X(H00Y)
2.b Secondary CH2 refined with riding coordinates:
 C00N(H00K,H00L), C00Y(H00Z,H), C010(H01A,H01B), C011(H01C,H01D), C015(H01K,
 H01L), C019(H01M,H01N)
2.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00E(H00E), C00H(H00H), C00J(H3AA), C00M(H00M), C00Q(H00Q),
 C00T(H00T), C00U(H00U), C012(H012), C018(H018), C01B(H4AA), C01E(H5AA),
 C01F(H8AA), C01H(H6AA), C01J(H9AA), C01K(H0BA), C01L(H1BA), C01M(H7AA),
 C01Q(H2BA), C01R(H3BA)
2.d Idealised Me refined as rotating group:
 C00G(H00A,H00C,H00F), C00L(H00G,H00I,H00J), C00S(H00N,H00R,H00S), C00W(H00V,
 H00W,H00X), C00Z(H00,HA,HB), C013(H01E,H01F,H01G), C014(H01H,H01I,H01J),
 C01A(H01O,H01P,H01Q), C01C(H01R,H01S,H01T), C01D(H01U,H01V,H01W), C01G(H01X,
 H01Y,HC), C01I(H01Z,HD,HE), C01N(H01,HF,HG), C01O(H0AA,HH,HI), C01P(H1AA,HJ,
 HK), C01S(H2AA,HL,HM)
;
_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 2.451
_oxdiff_exptl_absorpt_empirical_full_min 0.505