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_7049794
_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 N4 Rh, C32 H12 B F24, 1(C5 H12)'
_chemical_formula_sum            'C72 H70 B F24 N4 Rh'
_chemical_formula_weight         1561.04
_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                 106.9706(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.49982(19)
_cell_length_b                   18.08188(17)
_cell_length_c                   24.0311(3)
_cell_measurement_reflns_used    14637
_cell_measurement_temperature    150.04(18)
_cell_measurement_theta_max      75.7460
_cell_measurement_theta_min      3.6600
_cell_volume                     7273.03(14)
_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      150.04(18)
_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     81.00 124.00   1.00    3.00    --   42.66 178.00  30.00   43
  2  \w     60.00 121.00   1.00    3.00    --   42.66 178.00-120.00   61
  3  \w    -41.00  36.00   1.00    3.00    --  -42.66  19.00  60.00   77
  4  \w    -49.00  29.00   1.00    3.00    --  -42.66  38.00 -60.00   78
  5  \w    146.00 172.00   1.00   10.00    --  111.00 125.00  90.00   26
  6  \w    123.00 170.00   1.00   10.00    --  111.00 115.00 -54.00   47
  7  \w     81.00 174.00   1.00   10.00    --  111.00  15.00 150.00   93
  8  \w     82.00 107.00   1.00   10.00    --  111.00 -95.00 -60.00   25
  9  \w     96.00 121.00   1.00   10.00    --  111.00-125.00 -60.00   25
 10  \w     76.00 118.00   1.00   10.00    --  111.00-125.00-150.00   42
 11  \w     57.00  97.00   1.00   10.00    --  111.00 -45.00-180.00   40
 12  \w     43.00  89.00   1.00   10.00    --  111.00 -30.00-180.00   46
 13  \w     38.00 139.00   1.00   10.00    --  111.00 -77.00-150.00  101
 14  \w     49.00  89.00   1.00   10.00    --  111.00 -30.00   0.00   40
 15  \w     51.00 108.00   1.00   10.00    --  111.00 -95.00  30.00   57
 16  \w     42.00  68.00   1.00   10.00    --  111.00 -45.00 120.00   26
 17  \w     37.00  90.00   1.00   10.00    --  111.00 -30.00  60.00   53
 18  \w     37.00  64.00   1.00   10.00    --  111.00 -95.00  60.00   27
 19  \w     36.00  89.00   1.00   10.00    --  111.00 -30.00 -60.00   53
 20  \w     32.00  60.00   1.00   10.00    --  111.00 -95.00 -60.00   28
 21  \w     42.00  68.00   1.00   10.00    --  111.00-125.00 -60.00   26
 22  \w     42.00  71.00   1.00   10.00    --  111.00-125.00-150.00   29
;
_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      0.0505578000
_diffrn_orient_matrix_UB_12      0.0144484000
_diffrn_orient_matrix_UB_13      -0.0417107000
_diffrn_orient_matrix_UB_21      -0.0215359000
_diffrn_orient_matrix_UB_22      0.0827666000
_diffrn_orient_matrix_UB_23      -0.0017537000
_diffrn_orient_matrix_UB_31      0.0738783000
_diffrn_orient_matrix_UB_32      0.0142494000
_diffrn_orient_matrix_UB_33      0.0523791000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47642
_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         76.164
_diffrn_reflns_theta_min         3.598
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79202
_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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       plate
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.198
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         15081
_refine_ls_number_restraints     589
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0723P)^2^+6.2268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11420
_reflns_number_total             15081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00971j2.cif
_cod_data_source_block           143amm18
_cod_depositor_comments
'Adding full bibliography for 7049789--7049794.cif.'
_cod_original_cell_volume        7273.01(14)
_cod_database_code               7049794
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C54 H66 Rh1 B1 F24 N3 O2'
_shelx_estimated_absorpt_t_max   0.604
_shelx_estimated_absorpt_t_min   0.568
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C69-C68 = C69A-C68A = C70-C69 = C70A-C69A = C71-C70 = C71A-C70A = C72A-C71A =
 C72-C71
 1.51 with sigma of 0.01
 F4-F5 \\sim F4-F6 \\sim F5-F6 \\sim F4A-F5A \\sim F4A-F6A \\sim F5A-F6A
 with sigma of 0.04
 F22-F23 \\sim F22-F24 \\sim F23-F24 \\sim F23A-F22A \\sim F23A-F24A \\sim
F22A-F24A
 with sigma of 0.04
 C67-F22 \\sim C67-F23 \\sim C67-F24 \\sim C67-F23A \\sim C67-F22A \\sim
C67-F24A
 with sigma of 0.02
 C43-F4 \\sim C43-F5 \\sim C43-F6 \\sim C43-F4A \\sim C43-F5A \\sim C43-F6A
 with sigma of 0.02
 F7-F8 \\sim F7-F9 \\sim F8-F9 \\sim F9A-F8A \\sim F9A-F7A \\sim F8A-F7A
 with sigma of 0.04
 C51-F7 \\sim C51-F8 \\sim C51-F9 \\sim C51-F9A \\sim C51-F8A \\sim C51-F7A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C67 \\sim F22 \\sim F23 \\sim F24 \\sim F24A \\sim F22A \\sim F23A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C43 \\sim F4 \\sim F5 \\sim F6 \\sim F4A \\sim F5A \\sim F6A: 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: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C68A \\sim C69A \\sim C70A
\\sim C71A \\sim C72A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
4. Rigid body (RIGU) restrains
 C67, F22, F23, F24, F24A, F22A, F23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, F4, F5, F6, F4A, F5A, F6A
 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
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C68, C69, C70, C71, C72, C68A, C69A, C70A, C71A, C72A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(F24A)=Sof(F22A)=Sof(F23A)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
 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)=1-FVAR(4)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=
 Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=
 Sof(H72C)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C69A(H69C,H69D), C70A(H70C,
 H70D), C71A(H71C,H71D)
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), C57(H57), C37(H37), C39(H39), C41(H41), C49(H49), C47(H47), C45(H45),
  C53(H53), C55(H55), 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), C68(H68A,
 H68B,H68C), C72(H72A,H72B,H72C), C68A(H68D,H68E,H68F), C72A(H72D,H72E,H72F)
;
_shelx_res_checksum              22507
_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 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.783