A d<sup>10</sup> Ag(i) amine-borane σ-complex and comparison with a d<sup>8</sup> Rh(i) analogue: structures on the η<sup>1</sup> to η<sup>2</sup>:η<sup>2</sup> continuum.
Johnson, Alice; Martínez-Martínez, Antonio J; Macgregor, Stuart A.; Weller, Andrew S.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9776–9781; doi:10.1039/c9dt00971j

data_7049790
_publ_section_title
;
 A d<sup>10</sup> Ag(i) amine-borane \s-complex and comparison with a
 d<sup>8</sup> Rh(i) analogue: structures on the \h<sup>1</sup> to
 \h<sup>2</sup>:\h<sup>2</sup> continuum.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9776
_journal_page_last               9781
_journal_paper_doi               10.1039/c9dt00971j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H43 Ag F3 N3 O3 S'
_chemical_formula_sum            'C34 H43 Ag F3 N3 O3 S'
_chemical_formula_weight         738.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-04 deposited with the CCDC.    2019-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.758(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.81000(10)
_cell_length_b                   14.6740(2)
_cell_length_c                   12.8614(2)
_cell_measurement_reflns_used    13118
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.4100
_cell_measurement_theta_min      5.6140
_cell_volume                     1753.09(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -38.00   0.00   1.00    1.00    --    0.00  57.00-180.00   38
  2  \w     27.00  91.00   1.00    1.00    --    0.00  57.00-180.00   64
  3  \w   -149.00 -80.00   1.00    4.00    --  -60.50 -94.00  30.00   69
  4  \w   -134.00 -97.00   1.00    4.00    --  -60.50 -94.00 -60.00   37
  5  \w   -127.00 -99.00   1.00    4.00    --  -60.50 -94.00 -90.00   28
  6  \w    -24.00  91.00   1.00    4.00    --   60.50 -30.00-120.00  115
  7  \w    125.00 151.00   1.00    4.00    --   60.50 125.00  90.00   26
  8  \w     29.00 107.00   1.00    4.00    --   60.50-125.00-120.00   78
  9  \w     79.00 167.00   1.00    6.00    --  121.00  77.00 -30.00   88
 10  \w     58.00  84.00   1.00    6.00    --  121.00 -37.00  60.00   26
 11  \w     82.00 178.00   1.00    6.00    --  121.00  77.00  90.00   96
 12  \w    100.00 143.00   1.00    6.00    --  121.00 111.00  90.00   43
 13  \w     49.00  81.00   1.00    6.00    --  121.00 -91.00-150.00   32
 14  \w     91.00 158.00   1.00    6.00    --  121.00 -91.00-150.00   67
 15  \w     30.00  76.00   1.00    6.00    --  121.00-111.00 -60.00   46
 16  \w     50.00  94.00   1.00    6.00    --  121.00 -25.00-180.00   44
 17  \w     35.00 105.00   1.00    6.00    --  121.00-111.00-150.00   70
 18  \w    126.00 176.00   1.00    6.00    --  121.00 111.00  60.00   50
 19  \w     92.00 156.00   1.00    6.00    --  121.00  63.00  30.00   64
 20  \w     18.00  50.00   1.00    1.00    --    0.00 -99.00   0.00   32
 21  \w     10.00  43.00   1.00    1.00    --    0.00 -99.00  60.00   33
 22  \w      1.00  26.00   1.00    1.00    --    0.00 -99.00-180.00   25
 23  \w      6.00  31.00   1.00    4.00    --  -60.50  45.00-180.00   25
 24  \w   -137.00-107.00   1.00    4.00    --  -60.50 -94.00  90.00   30
 25  \w    -54.00 -28.00   1.00    4.00    --  -60.50  45.00-180.00   26
 26  \w    116.00 151.00   1.00    4.00    --   60.50  45.00 150.00   35
 27  \w     30.00  84.00   1.00    4.00    --   60.50-125.00  60.00   54
 28  \w     95.00 121.00   1.00    4.00    --   60.50 125.00-180.00   26
 29  \w     27.00 114.00   1.00    4.00    --   60.50  45.00 150.00   87
 30  \w     14.00  93.00   1.00    4.00    --   60.50 -94.00  90.00   79
 31  \w    116.00 142.00   1.00    4.00    --   60.50 125.00  30.00   26
 32  \w     80.00 112.00   1.00    6.00    --  121.00-111.00-120.00   32
 33  \w    121.00 156.00   1.00    6.00    --  121.00  50.00  60.00   35
 34  \w     48.00  76.00   1.00    6.00    --  121.00-111.00-120.00   28
 35  \w     86.00 112.00   1.00    6.00    --  121.00-111.00 -30.00   26
 36  \w     84.00 111.00   1.00    6.00    --  121.00-111.00 -60.00   27
 37  \w    101.00 161.00   1.00    6.00    --  121.00 111.00-120.00   60
 38  \w     46.00 111.00   1.00    6.00    --  121.00-111.00-180.00   65
 39  \w    120.00 147.00   1.00    6.00    --  121.00  77.00 -90.00   27
 40  \w     78.00 112.00   1.00    6.00    --  121.00  77.00 -90.00   34
 41  \w     63.00  94.00   1.00    6.00    --  121.00 -50.00 -90.00   31
 42  \w     87.00 175.00   1.00    6.00    --  121.00  77.00   0.00   88
 43  \w     30.00  68.00   1.00    6.00    --  121.00 -25.00   0.00   38
 44  \w     38.00  86.00   1.00    6.00    --  121.00-111.00  60.00   48
 45  \w     67.00 112.00   1.00    6.00    --  121.00-111.00  30.00   45
 46  \w    132.00 158.00   1.00    6.00    --  121.00 -91.00 120.00   26
 47  \w     80.00 165.00   1.00    6.00    --  121.00  63.00 -60.00   85
 48  \w     62.00  88.00   1.00    6.00    --  121.00 -91.00 120.00   26
 49  \w      8.00  35.00   1.00    1.00    --    0.00 -99.00  90.00   27
 50  \w      4.00  48.00   1.00    1.00    --    0.00 -99.00-150.00   44
 51  \w     14.00  72.00   1.00    4.00    --   60.50  15.00 120.00   58
 52  \w     95.00 121.00   1.00    4.00    --   60.50  15.00 120.00   26
 53  \w    142.00 173.00   1.00    6.00    --  121.00 111.00-180.00   31
 54  \w    102.00 133.00   1.00    6.00    --  121.00 111.00 -60.00   31
 55  \w     44.00  70.00   1.00    6.00    --  121.00 -37.00 -90.00   26
 56  \w     65.00  92.00   1.00    6.00    --  121.00 -37.00   0.00   27
 57  \w     37.00  71.00   1.00    6.00    --  121.00 -50.00 -30.00   34
 58  \w    114.00 140.00   1.00    6.00    --  121.00 178.00-180.00   26
 59  \w     82.00 109.00   1.00    6.00    --  121.00 178.00-180.00   27
 60  \w     72.00 105.00   1.00    6.00    --  121.00-111.00 120.00   33
 61  \w     85.00 112.00   1.00    6.00    --  121.00-111.00 150.00   27
 62  \w    101.00 128.00   1.00    6.00    --  121.00-140.00 103.12   27
 63  \w    -90.00 -53.00   1.00    1.00    --    0.00 -37.00  90.00   37
 64  \w     -7.00  27.00   1.00    1.00    --    0.00 -37.00  90.00   34
 65  \w    -37.00 -10.00   1.00    1.00    --    0.00 -37.00  90.00   27
 66  \w    -68.00 -37.00   1.00    1.00    --    0.00 178.00-120.00   31
 67  \w    -44.00 -18.00   1.00    1.00    --   18.00 119.00-167.58   26
 68  \w    -49.00 -24.00   1.00    4.00    --   42.00 162.00 137.06   25
 69  \w      1.00  26.00   1.00    4.00    --   50.00  93.00 -98.34   25
 70  \w      9.00  34.00   1.00    4.00    --   54.00  85.00  10.64   25
 71  \w      9.00  34.00   1.00    4.00    --   54.00  86.00 176.95   25
 72  \w      8.00  33.00   1.00    4.00    --   54.00  87.00  47.07   25
 73  \w     16.00  43.00   1.00    4.00    --   60.50  81.00  45.27   27
 74  \w     16.00  42.00   1.00    4.00    --   60.50  82.00 -41.06   26
 75  \w     18.00  43.00   1.00    4.00    --   62.00  80.00 -88.91   25
 76  \w     18.00  43.00   1.00    4.00    --   62.00  80.00  93.95   25
 77  \w     32.00 115.00   1.00    4.00    --   66.00  77.00 -34.76   83
 78  \w     81.00 126.00   1.00    4.00    --   66.00  71.00-148.08   45
 79  \w     92.00 118.00   1.00    4.00    --   66.00  72.00 -96.04   26
 80  \w     23.00  58.00   1.00    4.00    --   66.00  71.00-148.08   35
 81  \w     24.00  58.00   1.00    4.00    --   66.00  72.00 -96.04   34
 82  \w     26.00  55.00   1.00    4.00    --   70.00  65.00 155.82   29
 83  \w     27.00  67.00   1.00    4.00    --   70.00  77.00  75.63   40
 84  \w     94.00 144.00   1.00    4.00    --   70.00  65.00 155.82   50
;
_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      -0.0374601000
_diffrn_orient_matrix_UB_12      0.0099815000
_diffrn_orient_matrix_UB_13      -0.1253067000
_diffrn_orient_matrix_UB_21      0.0456691000
_diffrn_orient_matrix_UB_22      -0.0995945000
_diffrn_orient_matrix_UB_23      -0.0075949000
_diffrn_orient_matrix_UB_31      -0.1549581000
_diffrn_orient_matrix_UB_32      -0.0317529000
_diffrn_orient_matrix_UB_33      -0.0154872000
_diffrn_radiation_monochromator  mirror
_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     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23626
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.736
_diffrn_reflns_theta_min         3.629
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.611
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       needle
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 3255 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0506P)^2^+0.3994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                7081
_reflns_number_total             7285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00971j2.cif
_cod_data_source_block           141amm18re
_cod_depositor_comments
'Adding full bibliography for 7049789--7049794.cif.'
_cod_original_cell_volume        1753.09(4)
_cod_database_code               7049790
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C54 H23 Ag1 N3 F3 S1 O3'
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.432
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              98913
_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 1.663
_oxdiff_exptl_absorpt_empirical_full_min 0.636