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_1557458
_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         'C30 H44 Ag Li N2 O3, 2(C6 H6)'
_chemical_formula_sum            'C42 H56 Ag Li N2 O3'
_chemical_formula_weight         751.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 93.742(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4986(2)
_cell_length_b                   14.8962(2)
_cell_length_c                   21.7554(4)
_cell_measurement_reflns_used    16840
_cell_measurement_temperature    90
_cell_measurement_theta_max      77.1570
_cell_measurement_theta_min      3.5550
_cell_volume                     4041.82(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (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      90
_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 1.000
_diffrn_measured_fraction_theta_max 0.969
_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    -44.00 112.00   0.50    0.50    --   39.95 -16.00  19.00  312
  2  \w     33.00 118.00   0.50    1.80    --  115.57 -16.00  19.00  170
  3  \w     75.00 103.00   0.50    1.80    --  115.57 -94.00   0.00   56
  4  \w     49.00  77.00   0.50    1.80    --  115.57 -45.00 -30.00   56
  5  \w     42.00  99.00   0.50    1.80    --  115.57 -94.00 -90.00  114
  6  \w     66.00 108.00   0.50    1.80    --  115.57 -94.00-150.00   84
  7  \w     58.00  84.00   0.50    1.80    --  115.57 -94.00-180.00   52
  8  \w     33.00  58.00   0.50    1.80    --  115.57 -30.00-150.00   50
  9  \w     37.00  72.00   0.50    1.80    --  115.57 -45.00-120.00   70
 10  \w    106.00 177.00   0.50    1.80    --  115.57  16.00-171.00  142
 11  \w     44.00  72.00   0.50    1.80    --  115.57 -94.00   0.00   56
 12  \w     41.00  98.00   0.50    1.80    --  115.57-125.00   0.00  114
 13  \w     34.00  64.00   0.50    1.80    --  115.57 -30.00   0.00   60
 14  \w     40.00  77.00   0.50    1.80    --  115.57 -45.00   0.00   74
 15  \w     40.00  79.00   0.50    1.80    --  115.57 -45.00 -60.00   78
 16  \w     35.00  68.00   0.50    1.80    --  115.57 -30.00 -90.00   66
 17  \w     34.00  68.00   0.50    1.80    --  115.57 -30.00-120.00   68
 18  \w    -71.00 -46.00   0.50    0.50    --  -39.95 -16.00  19.00   50
 19  \w    -64.00  -3.00   0.50    1.80    --  -84.50  30.00 -30.00  122
 20  \w   -106.00 -81.00   0.50    1.80    --  -84.50  16.00-171.00   50
 21  \w   -117.00 -78.00   0.50    0.50    --  -39.95  16.00-171.00   78
 22  \w   -143.00 -90.00   0.50    1.80    --  -84.50 -16.00  19.00  106
 23  \w   -114.00 -10.00   0.50    1.80    --  -84.50  61.00  30.00  208
 24  \w   -164.00 -80.00   0.50    1.80    --  -84.50 -94.00 150.00  168
 25  \w   -123.00 -38.00   0.50    0.50    --  -39.95-178.00 120.00  170
;
_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      -0.1025727000
_diffrn_orient_matrix_UB_12      -0.0055106000
_diffrn_orient_matrix_UB_13      0.0354156000
_diffrn_orient_matrix_UB_21      -0.0683643000
_diffrn_orient_matrix_UB_22      0.0208910000
_diffrn_orient_matrix_UB_23      -0.0598020000
_diffrn_orient_matrix_UB_31      -0.0084441000
_diffrn_orient_matrix_UB_32      -0.1011134000
_diffrn_orient_matrix_UB_33      -0.0143263000
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27075
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.112
_diffrn_reflns_theta_min         3.599
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              PhotonJet-S
_exptl_absorpt_coefficient_mu    4.283
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.581
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         8303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7705
_reflns_number_total             8303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06060j2.cif
_cod_data_source_block           exp_28
_cod_depositor_comments
'Adding full bibliography for 1557456--1557459.cif.'
_cod_database_code               1557458
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C36H50Ag1Li1N2O3
_reflns_odcompleteness_completeness 99.99
_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:
 C00F(H00F), C00G(H00G), C00J(H00J), C00N(H00O)
2.b Secondary CH2 refined with riding coordinates:
 C00Q(H00R,H00S), C00V(H00,HC), C012(H01A,H01B), C015(H01C,H01D)
2.c Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00E(H00E), C00H(H00H), C00I(H00I), C00L(H00L), C00O(H00P),
 C00P(H00Q), C00R(H00T), C00Y(H2AA), C00Z(H3AA), C010(H010), C011(H011),
 C013(H013), C014(H014), C017(H017), C018(H018), C019(H019), C01A(H01H),
 C01B(H01I), C01C(H01J)
2.d Idealised Me refined as rotating group:
 C00K(H00A,H00B,H00D), C00M(H00K,H00M,H00N), C00S(H00U,H00V,H00W), C00T(H00X,
 H00Y,H), C00U(H00Z,HA,HB), C00W(H0AA,HD,HE), C00X(H1AA,HF,HG), C016(H01E,H01F,
 H01G)
;
_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 2.233
_oxdiff_exptl_absorpt_empirical_full_min 0.683