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_7049793
_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         'C36 H55 Ag B N4, C32 H12 B F24'
_chemical_formula_sum            'C68 H67 Ag B2 F24 N4'
_chemical_formula_weight         1525.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                88.4148(13)
_cell_angle_beta                 74.0062(14)
_cell_angle_gamma                78.2248(14)
_cell_formula_units_Z            2
_cell_length_a                   14.4114(2)
_cell_length_b                   15.6413(3)
_cell_length_c                   16.8798(3)
_cell_measurement_reflns_used    51261
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      76.1310
_cell_measurement_theta_min      3.8460
_cell_volume                     3579.02(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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      150.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -30.00  29.00   1.00    1.00    --  -42.66  38.00 -30.00   59
  2  \w    -18.00  30.00   1.00    1.00    --  -42.66  38.00-120.00   48
  3  \w    -22.00  26.00   1.00    1.00    --  -42.66  38.00  30.00   48
  4  \w    -50.00 -25.00   1.00    1.00    --  -42.66  38.00-120.00   25
  5  \w   -120.00  -8.00   1.00    1.00    --  -42.66 -19.00  60.00  112
  6  \w     75.00 117.00   1.00    1.00    --   42.66 178.00 -30.00   42
  7  \w     84.00 129.00   1.00    1.00    --   42.66 178.00-150.00   45
  8  \w     94.00 129.00   1.00    1.00    --   42.66 178.00 120.00   35
  9  \w    113.00 178.00   1.00    4.00    --  111.00  15.00-180.00   65
 10  \w    107.00 138.00   1.00    4.00    --  111.00 -77.00-150.00   31
 11  \w     92.00 118.00   1.00    4.00    --  111.00-125.00-120.00   26
 12  \w     90.00 118.00   1.00    4.00    --  111.00-125.00-180.00   28
 13  \w     52.00  96.00   1.00    4.00    --  111.00 -95.00 -60.00   44
 14  \w     72.00 121.00   1.00    4.00    --  111.00-123.00 -50.73   49
 15  \w     68.00 120.00   1.00    4.00    --  111.00-125.00  30.00   52
 16  \w    104.00 134.00   1.00    4.00    --  111.00 -77.00  90.00   30
 17  \w     94.00 141.00   1.00    4.00    --  111.00 -15.00 150.00   47
 18  \w    123.00 169.00   1.00    4.00    --  111.00  30.00 120.00   46
 19  \w     77.00 165.00   1.00    4.00    --  111.00  15.00  90.00   88
 20  \w     66.00 119.00   1.00    4.00    --  111.00-125.00 120.00   53
 21  \w     59.00 128.00   1.00    4.00    --  111.00 -61.00  60.00   69
 22  \w     50.00  76.00   1.00    4.00    --  111.00 -77.00  90.00   26
 23  \w     41.00 109.00   1.00    4.00    --  111.00 -95.00  60.00   68
 24  \w     43.00  86.00   1.00    4.00    --  111.00 -15.00 150.00   43
 25  \w     41.00  67.00   1.00    4.00    --  111.00 -45.00 150.00   26
 26  \w     36.00  88.00   1.00    4.00    --  111.00 -30.00  90.00   52
 27  \w     41.00  81.00   1.00    4.00    --  111.00 -45.00   0.00   40
 28  \w     40.00  89.00   1.00    4.00    --  111.00 -30.00 -90.00   49
 29  \w     55.00  94.00   1.00    4.00    --  111.00 -45.00-180.00   39
 30  \w     41.00 100.00   1.00    4.00    --  111.00 -77.00-150.00   59
 31  \w     46.00  72.00   1.00    4.00    --  111.00-125.00-180.00   26
 32  \w     43.00  69.00   1.00    4.00    --  111.00-125.00-120.00   26
 33  \w     40.00  68.00   1.00    4.00    --  111.00 -45.00 -90.00   28
 34  \w     36.00  86.00   1.00    4.00    --  111.00 -30.00-150.00   50
 35  \w     39.00  65.00   1.00    4.00    --  111.00-125.00  30.00   26
 36  \w     30.00  98.00   1.00    4.00    --  111.00 -95.00  30.00   68
 37  \w     39.00  91.00   1.00    4.00    --  111.00 -30.00  30.00   52
 38  \w      7.00  32.00   1.00    1.00    --   42.00  89.00-149.12   25
 39  \w      8.00  33.00   1.00    1.00    --   42.00  86.00  83.37   25
 40  \w      9.00  38.00   1.00    1.00    --   42.00  83.00 -36.50   29
 41  \w    -59.00 -20.00   1.00    1.00    --  -42.66 -38.00   0.00   39
 42  \w   -113.00 -30.00   1.00    1.00    --  -42.66 -38.00-150.00   83
 43  \w    -49.00  17.00   1.00    1.00    --  -42.66  38.00-180.00   66
 44  \w   -104.00 -70.00   1.00    1.00    --  -42.66 -38.00   0.00   34
 45  \w     79.00 106.00   1.00    1.00    --   42.66  57.00-150.00   27
 46  \w     17.00  42.00   1.00    1.00    --   42.66  57.00-150.00   25
 47  \w     17.00  43.00   1.00    1.00    --   50.00  82.00 -48.58   26
 48  \w     18.00  43.00   1.00    1.00    --   50.00  81.00  97.03   25
 49  \w     18.00  43.00   1.00    1.00    --   50.00  81.00-137.88   25
 50  \w     22.00  47.00   1.00    1.00    --   54.00  78.00 -53.85   25
 51  \w     23.00  49.00   1.00    1.00    --   54.00  78.00  51.48   26
 52  \w     28.00  54.00   1.00    1.00    --   58.00  77.00 129.82   26
 53  \w     35.00  61.00   1.00    1.00    --   66.00  77.00-155.19   26
 54  \w    114.00 140.00   1.00    1.00    --   66.00  77.00-155.19   26
 55  \w    111.00 137.00   1.00    1.00    --   66.00  75.00-105.18   26
 56  \w     35.00  61.00   1.00    1.00    --   66.00  75.00-105.18   26
 57  \w     39.00  65.00   1.00    1.00    --   70.00  77.00 -28.04   26
 58  \w     40.00  69.00   1.00    1.00    --   70.00  77.00-134.21   29
 59  \w     39.00  65.00   1.00    1.00    --   70.00  77.00  -5.08   26
 60  \w     39.00  65.00   1.00    1.00    --   70.00  75.00  92.44   26
 61  \w     39.00  65.00   1.00    1.00    --   70.00  76.00 -60.04   26
 62  \w     39.00  65.00   1.00    1.00    --   70.00  77.00 142.35   26
 63  \w     43.00  69.00   1.00    1.00    --   74.00  77.00  15.36   26
 64  \w     43.00  69.00   1.00    1.00    --   74.00  77.00 -92.83   26
 65  \w     43.00  69.00   1.00    1.00    --   74.00  75.00 120.21   26
 66  \w     43.00  69.00   1.00    1.00    --   74.00  77.00 159.96   26
 67  \w     48.00  74.00   1.00    4.00    --   78.00  73.00  49.39   26
 68  \w     48.00  74.00   1.00    4.00    --   78.00  71.00 174.62   26
 69  \w     54.00  80.00   1.00    4.00    --   82.00  64.00-109.92   26
 70  \w     56.00  82.00   1.00    4.00    --   86.00  71.00 -30.44   26
 71  \w     58.00  84.00   1.00    4.00    --   86.00  66.00  10.20   26
 72  \w     57.00  87.00   1.00    4.00    --   86.00  67.00  67.04   30
 73  \w     55.00  81.00   1.00    4.00    --   86.00  74.00 -83.84   26
 74  \w     60.00  87.00   1.00    4.00    --   90.00  71.00-176.71   27
 75  \w     64.00  90.00   1.00    4.00    --   94.00  71.00  95.88   26
 76  \w     71.00  96.00   1.00    4.00    --  102.00  76.00 -79.51   25
 77  \w     78.00 104.00   1.00    4.00    --  106.00  66.00 -46.79   26
 78  \w     83.00 117.00   1.00    4.00    --  111.00  61.00 150.00   34
 79  \w    128.00 155.00   1.00    4.00    --  111.00  77.00 -30.00   27
 80  \w     83.00 154.00   1.00    4.00    --  111.00  61.00-120.00   71
 81  \w     81.00 123.00   1.00    4.00    --  111.00  77.00 -30.00   42
 82  \w     80.00 120.00   1.00    4.00    --  111.00  77.00  68.69   40
 83  \w     80.00 167.00   1.00    4.00    --  111.00  77.00-180.00   87
 84  \w     81.00 141.00   1.00    4.00    --  111.00  71.00   2.96   60
 85  \w     83.00 167.00   1.00    4.00    --  111.00  61.00 -60.00   84
 86  \w     84.00 124.00   1.00    4.00    --  111.00  61.00  60.00   40
 87  \w    143.00 169.00   1.00    4.00    --  111.00  77.00 150.00   26
 88  \w     80.00 128.00   1.00    4.00    --  111.00  77.00 150.00   48
 89  \w     83.00 143.00   1.00    4.00    --  111.00  61.00-150.00   60
 90  \w     83.00 160.00   1.00    4.00    --  111.00  61.00 -90.00   77
 91  \w     84.00 113.00   1.00    4.00    --  111.00  61.00  30.00   29
 92  \w     80.00 107.00   1.00    4.00    --  111.00  77.00 120.00   27
 93  \w    128.00 158.00   1.00    4.00    --  111.00  61.00 -30.00   30
 94  \w     83.00 123.00   1.00    4.00    --  111.00  61.00 -30.00   40
 95  \w     80.00 119.00   1.00    4.00    --  111.00  77.00  90.00   39
 96  \w    139.00 165.00   1.00    4.00    --  111.00  77.00-120.00   26
 97  \w     80.00 106.00   1.00    4.00    --  111.00  77.00-120.00   26
 98  \w     80.00 107.00   1.00    4.00    --  111.00  77.00  30.00   27
 99  \w     80.00 153.00   1.00    4.00    --  111.00  77.00-150.00   73
100  \w     84.00 117.00   1.00    4.00    --  111.00  61.00 120.00   33
;
_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      -0.0793720000
_diffrn_orient_matrix_UB_12      0.0782733000
_diffrn_orient_matrix_UB_13      -0.0109138000
_diffrn_orient_matrix_UB_21      -0.0501277000
_diffrn_orient_matrix_UB_22      -0.0621642000
_diffrn_orient_matrix_UB_23      -0.0351205000
_diffrn_orient_matrix_UB_31      -0.0639756000
_diffrn_orient_matrix_UB_32      -0.0118613000
_diffrn_orient_matrix_UB_33      0.0875766000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            90787
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.319
_diffrn_reflns_theta_min         3.626
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         14883
_refine_ls_number_restraints     1176
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0464P)^2^+1.8775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14235
_reflns_number_total             14883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00971j2.cif
_cod_data_source_block           171amm18
_cod_depositor_comments
'Adding full bibliography for 7049789--7049794.cif.'
_cod_original_cell_volume        3579.03(10)
_cod_database_code               7049793
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C54 H66 N4 Ag1 F24 B2'
_shelx_estimated_absorpt_t_max   0.664
_shelx_estimated_absorpt_t_min   0.597
_reflns_odcompleteness_completeness 99.90
_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. Restrained distances
 F8-F9 \\sim F8-F7 \\sim F9-F7 \\sim F7A-F9A \\sim F7A-F8A \\sim F9A-F8A
 with sigma of 0.04
 C51-F8 \\sim C51-F9 \\sim C51-F7 \\sim C51-F7A \\sim C51-F9A \\sim C51-F8A
 with sigma of 0.02
 C35-C36 \\sim C35-C34 \\sim C35A-C36A \\sim C35A-C34A \\sim C36-C34 \\sim
C36A-C34A
 with sigma of 0.04
 N4-C35 \\sim N4-C35A \\sim N4-C36 \\sim N4-C36A \\sim N4-C34A \\sim N4-C34
 with sigma of 0.02
 F15-F14 \\sim F15-F13 \\sim F14-F13 \\sim F15A-F13A \\sim F15A-F14A \\sim
F13A-F14A
 with sigma of 0.04
 C59-F15 \\sim C59-F14 \\sim C59-F13 \\sim C59-F15A \\sim C59-F13A \\sim
C59-F14A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C51 \\sim F7 \\sim F8 \\sim F9 \\sim F7A \\sim F8A \\sim F9A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
N4 \\sim C34 \\sim C35 \\sim C36 \\sim C34A \\sim C35A \\sim C36A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F10 \\sim F11 \\sim F12
\\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23
\\sim F24 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43
\\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51
\\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59
\\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67
\\sim C68 \\sim B2 \\sim F7 \\sim F8 \\sim F9 \\sim F13 \\sim F14 \\sim F15:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C59 \\sim F13 \\sim F14 \\sim F15 \\sim F13A \\sim F14A \\sim F15A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C51, F7, F8, F9, F7A, F8A, F9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C34, C35, C36, C34A, C35A, C36A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F3, F4, F5, F6, F10, F11, F12, F16, F17, F18, F19, F20, F21, F22, F23,
  F24, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49, C50,
 C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64, C65, C66,
  C67, C68, B2, F7, F8, F9, F13, F14, F15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, F13, F14, F15, F13A, F14A, F15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(2)
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(3)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
6.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), C38(H38), C40(H40), C42(H42), C46(H46), C48(H48), C50(H50), C54(H54),
  C56(H56), C58(H58), C62(H62), C64(H64), C66(H66)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C34A(H34D,H34E,H34F), C35A(H35D,H35E,
 H35F), C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              60362
_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 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.840