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_7049789
_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 B N4 Rh, C32 H12 B F24, 0.25(C H2 Cl2), 0.5(C3 H7)'
_chemical_formula_sum            'C69.75 H71 B2 Cl0.5 F24 N4 Rh'
_chemical_formula_weight         1563.56
_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                85.814(2)
_cell_angle_beta                 81.7216(18)
_cell_angle_gamma                81.2409(16)
_cell_formula_units_Z            2
_cell_length_a                   12.9702(2)
_cell_length_b                   16.6310(4)
_cell_length_c                   17.7573(5)
_cell_measurement_reflns_used    19720
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      76.0380
_cell_measurement_theta_min      3.5540
_cell_volume                     3741.15(15)
_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      150.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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    -49.00  25.00   1.00    1.00    --  -42.53  38.00 -30.00   74
  2  \w    -39.00  26.00   1.00    1.00    --  -42.53  38.00-120.00   65
  3  \w    -28.00  28.00   1.00    1.00    --  -42.53  38.00-180.00   56
  4  \w     54.00  89.00   1.00    1.00    --   42.53-118.00 -46.00   35
  5  \w    -61.00 -25.00   1.00    1.00    --  -42.53  57.00  60.00   36
  6  \w   -113.00 -16.00   1.00    1.00    --  -42.53 -57.00  60.00   97
  7  \w   -119.00 -90.00   1.00    1.00    --  -42.53-178.00  90.00   29
  8  \w     39.00  66.00   1.00    4.00    --  111.00 -30.00  90.00   27
  9  \w     70.00  96.00   1.00    4.00    --  111.00 -45.00 120.00   26
 10  \w     85.00 154.00   1.00    4.00    --  111.00 -15.00 120.00   69
 11  \w    108.00 167.00   1.00    4.00    --  111.00  15.00  30.00   59
 12  \w    106.00 136.00   1.00    4.00    --  111.00 125.00  60.00   30
 13  \w    138.00 164.00   1.00    4.00    --  111.00 125.00  60.00   26
 14  \w     66.00 102.00   1.00    4.00    --  111.00  15.00  30.00   36
 15  \w     70.00 155.00   1.00    4.00    --  111.00 -15.00   0.00   85
 16  \w    116.00 141.00   1.00    4.00    --  111.00 -77.00-120.00   25
 17  \w     86.00 118.00   1.00    4.00    --  111.00-125.00 -60.00   32
 18  \w     78.00 121.00   1.00    4.00    --  111.00-125.00   0.00   43
 19  \w     86.00 138.00   1.00    4.00    --  111.00 -61.00  30.00   52
 20  \w     74.00 107.00   1.00    4.00    --  111.00-125.00 -90.00   33
 21  \w     85.00 119.00   1.00    4.00    --  111.00-125.00-180.00   34
 22  \w     53.00  79.00   1.00    4.00    --  111.00-125.00 -60.00   26
 23  \w     53.00  97.00   1.00    4.00    --  111.00-125.00 -30.00   44
 24  \w     60.00  94.00   1.00    4.00    --  111.00 -77.00  30.00   34
 25  \w     63.00 110.00   1.00    4.00    --  111.00-125.00  60.00   47
 26  \w     41.00 121.00   1.00    4.00    --  111.00-125.00  90.00   80
 27  \w     42.00  69.00   1.00    4.00    --  111.00 -30.00 -30.00   27
 28  \w     42.00  79.00   1.00    4.00    --  111.00 -30.00 -60.00   37
 29  \w     42.00  98.00   1.00    4.00    --  111.00 -45.00 -90.00   56
 30  \w     40.00  68.00   1.00    4.00    --  111.00 -45.00-180.00   28
 31  \w     38.00  81.00   1.00    4.00    --  111.00 -77.00-120.00   43
 32  \w     48.00  97.00   1.00    4.00    --  111.00-125.00-150.00   49
 33  \w     41.00 116.00   1.00    4.00    --  111.00-125.00-120.00   75
 34  \w     31.00  66.00   1.00    4.00    --  111.00 -15.00   0.00   35
 35  \w     42.00  79.00   1.00    4.00    --  111.00 -45.00  60.00   37
 36  \w     39.00 102.00   1.00    4.00    --  111.00 -95.00  90.00   63
 37  \w     31.00  80.00   1.00    4.00    --  111.00 -15.00 120.00   49
;
_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      0.0344589000
_diffrn_orient_matrix_UB_12      0.0032726000
_diffrn_orient_matrix_UB_13      -0.0867639000
_diffrn_orient_matrix_UB_21      0.0471935000
_diffrn_orient_matrix_UB_22      0.0785166000
_diffrn_orient_matrix_UB_23      0.0059651000
_diffrn_orient_matrix_UB_31      0.1062805000
_diffrn_orient_matrix_UB_32      -0.0513112000
_diffrn_orient_matrix_UB_33      0.0119779000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.343
_diffrn_reflns_theta_min         3.480
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75999
_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            plum
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       plate
_exptl_crystal_F_000             1594
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1278
_refine_ls_number_reflns         15487
_refine_ls_number_restraints     1556
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+1.7682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13951
_reflns_number_total             15487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00971j2.cif
_cod_data_source_block           154amm18
_cod_depositor_comments
'Adding full bibliography for 7049789--7049794.cif.'
_cod_original_cell_volume        3741.16(14)
_cod_original_formula_sum        'C69.75 H71 B2 Cl0.50 F24 N4 Rh'
_cod_database_code               7049789
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C54 H66 B2 Rh1 F24 N3'
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.567
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 B(H) groups, All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 F14-F15 \\sim F14-F13 \\sim F15-F13 \\sim F13A-F14A \\sim F13A-F15A \\sim
F14A-F15A
 with sigma of 0.04
 C59-F14 \\sim C59-F15 \\sim C59-F13 \\sim C59-F13A \\sim C59-F14A \\sim
C59-F15A
 with sigma of 0.02
 F21-F20 \\sim F21-F19 \\sim F20-F19 \\sim F19A-F21A \\sim F19A-F20A \\sim
F21A-F20A
 with sigma of 0.04
 C67-F21 \\sim C67-F20 \\sim C67-F19 \\sim C67-F19A \\sim C67-F21A \\sim
C67-F20A
 with sigma of 0.02
 F24-F23 \\sim F24-F22 \\sim F23-F22 \\sim F22A-F23A \\sim F22A-F24A \\sim
F23A-F24A
 with sigma of 0.04
 F9-F7 \\sim F9-F8 \\sim F7-F8 \\sim F7A-F9A \\sim F7A-F8A \\sim F9A-F8A \\sim
F7B-F9B \\sim F7B-F8B \\sim F9B-
 F8B
 with sigma of 0.04
 C51-F9 \\sim C51-F7 \\sim C51-F8 \\sim C51-F7A \\sim C51-F9A \\sim C51-F8A
\\sim C51-F7B \\sim C51-F9B ~
 C51-F8B
 with sigma of 0.02
 F17-F18 \\sim F17-F16 \\sim F18-F16 \\sim F16A-F17A \\sim F16A-F18A \\sim
F17A-F18A
 with sigma of 0.04
 C60-F17 \\sim C60-F18 \\sim C60-F16 \\sim C60-F16A \\sim C60-F17A \\sim
C60-F18A
 with sigma of 0.02
 F12-F11 \\sim F12-F10 \\sim F11-F10 \\sim F10A-F11A \\sim F10A-F12A \\sim
F11A-F12A
 with sigma of 0.04
 C52-F12 \\sim C52-F11 \\sim C52-F10 \\sim C52-F10A \\sim C52-F11A \\sim
C52-F12A
 with sigma of 0.02
 F2-F3 \\sim F2-F1 \\sim F3-F1 \\sim F1A-F3A \\sim F1A-F2A \\sim F3A-F2A \\sim
F1B-F3B \\sim F1B-F2B \\sim F3B-
 F2B
 with sigma of 0.04
 C43-F2 \\sim C43-F3 \\sim C43-F1 \\sim C43-F1A \\sim C43-F3A \\sim C43-F2A
\\sim C43-F1B \\sim C43-F3B ~
 C43-F2B
 with sigma of 0.02
 C68-F24 \\sim C68-F23 \\sim C68-F22 \\sim C68A-F22A \\sim C68A-F23A \\sim
C68A-F24A
 with sigma of 0.02
 C68-C65 \\sim C68A-C65
 with sigma of 0.02
 Cl2-C72 \\sim Cl1-C72
 with sigma of 0.02
 C70-C69 \\sim C71-C70
 with sigma of 0.02
 H1B-H1C \\sim H1B-H1CA \\sim H1A-H1C \\sim H1A-H1CA \\sim H1A-H1B
 with sigma of 0.02
 B1A-H1CA \\sim B1-H1C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
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
C67 \\sim F19 \\sim F20 \\sim F21 \\sim F19A \\sim F20A \\sim F21A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C51 \\sim F7 \\sim F8 \\sim F9 \\sim F7A \\sim F8A \\sim F9A \\sim F7B \\sim
F8B \\sim F9B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C60 \\sim F16 \\sim F17 \\sim F18 \\sim F16A \\sim F17A \\sim F18A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C52 \\sim F10 \\sim F11 \\sim F12 \\sim F10A \\sim F11A \\sim F12A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C43 \\sim F1 \\sim F2 \\sim F3 \\sim F1A \\sim F2A \\sim F3A \\sim F1B \\sim
F2B \\sim F3B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
F22A \\sim F23A \\sim F24A \\sim C68A \\sim F22 \\sim F23 \\sim F24 \\sim C68:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C69 \\sim C70 \\sim C71: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Cl1 \\sim Cl2 \\sim C72: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
N4 \\sim C34 \\sim C35 \\sim B1 \\sim N4A \\sim C34A \\sim C36A \\sim B1A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C68A) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C69) = Uanis(C70)
4. Rigid body (RIGU) restrains
 C67, F19, F20, F21, F19A, F20A, F21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, F7, F8, F9, F7A, F8A, F9A, F7B, F8B, F9B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C60, F16, F17, F18, F16A, F17A, F18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52, F10, F11, F12, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, F1, F2, F3, F1A, F2A, F3A, F1B, F2B, F3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F22A, F23A, F24A, C68A, F22, F23, F24, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C69, C70, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, Cl2, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C34, C35, C36, B1, N4A, C34A, C35A, C36A, B1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(F1)+Sof(F2)+Sof(F3)]+1*[Sof(F1A)+Sof(F2A)+Sof(F3A)]+1*[Sof(F1B)+
 Sof(F2B)+Sof(F3B)]=1 with esd of 0.0001
 1*[Sof(F7)+Sof(F8)+Sof(F9)]+1*[Sof(F7A)+Sof(F8A)+Sof(F9A)]+1*[Sof(F7B)+
 Sof(F8B)+Sof(F9B)]=1 with esd of 0.0001
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1)
 Sof(N4A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(H35D)=
 Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(B1A)=1-FVAR(2)
 Sof(N4)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(B1)=FVAR(2)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=Sof(C68)=1-FVAR(4)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=Sof(C68A)=FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(5)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(6)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=FVAR(7)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(8)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(9)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=FVAR(10)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(11)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(11)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(12)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(12)
 Fixed Sof: H1C(0.5) H1CA(0.5) Cl1(0.25) Cl2(0.25) C72(0.25) H72A(0.25)
 H72B(0.25) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C70(0.5) H70A(0.5) H70B(0.5)
 C71(0.5) H71A(0.5) H71B(0.5)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C72(H72A,H72B), C70(H70A,H70B), C71(H71A,H71B)
6.c 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.d 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), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C34A(H34D,H34E,H34F), C35A(H35D,H35E,H35F),
 C36A(H36D,H36E,H36F), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              59426
_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 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.590