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_7049791
_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         'C35 H46 Ag N4, C32 H12 B F24, 1(C5 H12)'
_chemical_formula_sum            'C72 H70 Ag B F24 N4'
_chemical_formula_weight         1566.00
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 107.0620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4613(2)
_cell_length_b                   17.68770(10)
_cell_length_c                   24.9895(2)
_cell_measurement_reflns_used    21935
_cell_measurement_temperature    150.01(12)
_cell_measurement_theta_max      76.1180
_cell_measurement_theta_min      3.6850
_cell_volume                     7378.33(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_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(12)
_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 0.989
_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    -46.00  26.00   1.00    1.00    --  -42.66  38.00  30.00   72
  2  \w     21.00  73.00   1.00    1.00    --   42.66  38.00 120.00   52
  3  \w    -72.00  26.00   1.00    1.00    --  -42.66  77.00-150.00   98
  4  \w     76.00 108.00   1.00    1.00    --   42.66 178.00-180.00   32
  5  \w     90.00 177.00   1.00    4.00    --  111.00  30.00  60.00   87
  6  \w    149.00 174.00   1.00    4.00    --  111.00  30.00 120.00   25
  7  \w     95.00 131.00   1.00    4.00    --  111.00  30.00 120.00   36
  8  \w     92.00 177.00   1.00    4.00    --  111.00  45.00 150.00   85
  9  \w     94.00 167.00   1.00    4.00    --  111.00 125.00 150.00   73
 10  \w    126.00 177.00   1.00    4.00    --  111.00  45.00 -90.00   51
 11  \w    133.00 158.00   1.00    4.00    --  111.00  45.00-180.00   25
 12  \w     89.00 115.00   1.00    4.00    --  111.00  45.00-180.00   26
 13  \w     57.00  83.00   1.00    4.00    --  111.00 -45.00-150.00   26
 14  \w     67.00  94.00   1.00    4.00    --  111.00 -50.00-121.00   27
 15  \w     39.00  81.00   1.00    4.00    --  111.00 -30.00-120.00   42
 16  \w     43.00  69.00   1.00    4.00    --  111.00 -61.00  30.00   26
 17  \w     87.00 131.00   1.00    4.00    --  111.00 -61.00  30.00   44
 18  \w     69.00 109.00   1.00    4.00    --  111.00 -95.00  60.00   40
 19  \w     61.00  86.00   1.00    4.00    --  111.00 -45.00 150.00   25
 20  \w     59.00  85.00   1.00    4.00    --  111.00 -95.00 120.00   26
 21  \w     44.00  89.00   1.00    4.00    --  111.00 -45.00  60.00   45
 22  \w     39.00  65.00   1.00    4.00    --  111.00 -95.00  60.00   26
 23  \w     33.00  75.00   1.00    4.00    --  111.00 -95.00  90.00   42
 24  \w   -121.00 -67.00   1.00    1.00    --  -42.66 -19.00 -60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0903238000
_diffrn_orient_matrix_UB_12      -0.0138760000
_diffrn_orient_matrix_UB_13      0.0265450000
_diffrn_orient_matrix_UB_21      -0.0077083000
_diffrn_orient_matrix_UB_22      -0.0772395000
_diffrn_orient_matrix_UB_23      -0.0296286000
_diffrn_orient_matrix_UB_31      0.0173651000
_diffrn_orient_matrix_UB_32      0.0377731000
_diffrn_orient_matrix_UB_33      -0.0507433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49302
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.301
_diffrn_reflns_theta_min         3.641
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         15294
_refine_ls_number_restraints     839
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+5.5481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13517
_reflns_number_total             15294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00971j2.cif
_cod_data_source_block           149amm18
_cod_depositor_comments
'Adding full bibliography for 7049789--7049794.cif.'
_cod_original_cell_volume        7378.32(12)
_cod_database_code               7049791
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C54 H66 Ag1 N3'
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.636
_reflns_odcompleteness_completeness 99.87
_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 C(H,H,H) groups
2. Restrained distances
 C69A-C68A = C70A-C69A = C71A-C70A = C72A-C71A
 1.52 with sigma of 0.01
 C68-C69 = C70-C69 = C70-C71 = C72-C71
 1.52 with sigma of 0.01
 F19A-F20A \\sim F19A-F21A \\sim F19-F20 \\sim F19-F21 \\sim F20-F21 \\sim
F20A-F21A
 with sigma of 0.04
 C66-F19A \\sim C66-F19 \\sim C66-F20 \\sim C66-F20A \\sim C66-F21 \\sim
C66-F21A
 with sigma of 0.02
 F8-F9 \\sim F8-F7 \\sim F9-F7 \\sim F8A-F9A \\sim F8A-F7A \\sim F9A-F7A
 with sigma of 0.04
 C50-F8 \\sim C50-F9 \\sim C50-F7 \\sim C50-F8A \\sim C50-F9A \\sim C50-F7A
 with sigma of 0.02
 F18A-F17A \\sim F18-F17 \\sim F17-F16 \\sim F17A-F16A
 with sigma of 0.04
 C59-F18A \\sim C59-F18 \\sim C59-F17 \\sim C59-F17A \\sim C59-F16 \\sim
C59-F16A
 with sigma of 0.02
 F23A-F22A \\sim F23A-F24A \\sim F23-F22 \\sim F23-F24 \\sim F22A-F24A \\sim
F22-F24
 with sigma of 0.04
 C67-F23A \\sim C67-F23 \\sim C67-F22A \\sim C67-F22 \\sim C67-F24A \\sim
C67-F24
 with sigma of 0.02
 F6-F4 \\sim F6-F5 \\sim F4-F5 \\sim F6A-F4A \\sim F6A-F5A \\sim F4A-F5A
 with sigma of 0.04
 C43-F6 \\sim C43-F4 \\sim C43-F5 \\sim C43-F6A \\sim C43-F4A \\sim C43-F5A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C68A \\sim C69A \\sim C70A \\sim C71A \\sim C72A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01
C71 \\sim C68 \\sim C69 \\sim C70 \\sim C72: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C66 \\sim F19A \\sim F20A \\sim F21A \\sim F19 \\sim F20 \\sim F21: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C50 \\sim F7A \\sim F8A \\sim F9A \\sim F7 \\sim F8 \\sim F9: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C59 \\sim F18A \\sim F16A \\sim F17A \\sim F18 \\sim F16 \\sim F17: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C67 \\sim F23A \\sim F22A \\sim F24A \\sim F23 \\sim F22 \\sim F24: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C43 \\sim F4A \\sim F5A \\sim F6A \\sim F4 \\sim F5 \\sim F6: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C68A) \\sim Ueq, Uanis(C69A) \\sim Ueq, Uanis(C70A) \\sim Ueq,
Uanis(C71A) \\sim Ueq, Uanis(C72A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C72) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 C68A, C69A, C70A, C71A, C72A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C71, C68, C69, C70, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C66, F19A, F20A, F21A, F19, F20, F21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C50, F7A, F8A, F9A, F7, F8, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, F18A, F16A, F17A, F18, F16, F17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C67, F23A, F22A, F24A, F23, F22, F24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, F4A, F5A, F6A, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(F18A)=Sof(F16A)=Sof(F17A)=1-FVAR(3)
 Sof(F18)=Sof(F16)=Sof(F17)=FVAR(3)
 Sof(F23A)=Sof(F22A)=Sof(F24A)=1-FVAR(4)
 Sof(F23)=Sof(F22)=Sof(F24)=FVAR(4)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(5)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(5)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=
 Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C72)=Sof(H72A)=Sof(H72B)=
 Sof(H72C)=1-FVAR(6)
 Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(C69A)=Sof(H69C)=Sof(H69D)=
 Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C71A)=Sof(H71C)=Sof(H71D)=Sof(C72A)=
 Sof(H72D)=Sof(H72E)=Sof(H72F)=FVAR(6)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C69A(H69C,H69D), C70A(H70C,H70D), C71A(H71C,H71D), C69(H69A,
 H69B), C70(H70A,H70B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C2(H2), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26), C37(H37), C39(H39), C41(H41), C45(H45), C47(H47), C49(H49), C53(H53),
  C55(H55), C57(H57), C61(H61), C63(H63), C65(H65)
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), C35(H35A,H35B,H35C),
 C68A(H68D,H68E,H68F), C72A(H72D,H72E,H72F), C68(H68A,H68B,H68C), C72(H72A,H72B,
 H72C)
;
_shelx_res_checksum              54584
_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 1.655
_oxdiff_exptl_absorpt_empirical_full_min 0.585