Strongly Coordinating Ligands to Form Weakly Coordinating yet Functional Organometallic Anions.
Fisher, Steven P.; McArthur, Scott G.; Tej, Varun; Lee, Sarah E.; Chan, Allen L.; Banda, Isaac; Gregory, Aaron; Berkley, Kevin; Tsay, Charlene; Rheingold, Arnold L.; Guisado-Barrios, Gregorio; Lavallo, Vincent; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10234

data_4133813
_publ_section_title
;
 Strongly Coordinating Ligands to Form Weakly Coordinating yet Functional
 Organometallic Anions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10234
_journal_year                    2019
_chemical_formula_moiety         'C11 H26 Ag Au B22 Br12 N2 O S'
_chemical_formula_sum            'C11 H26 Ag Au B22 Br12 N2 O S'
_chemical_formula_weight         1735.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                64.599(8)
_cell_angle_beta                 82.881(7)
_cell_angle_gamma                72.102(7)
_cell_formula_units_Z            2
_cell_length_a                   11.165(3)
_cell_length_b                   15.799(5)
_cell_length_c                   18.044(5)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    175
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.27
_cell_volume                     2735.9(14)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      175.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36548
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.607
_diffrn_reflns_theta_min         1.249
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.854
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0929 before and 0.0577 after correction. The Ratio of minimum to maximum transmission is 0.7092. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.749
_refine_diff_density_min         -1.612
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         12634
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0456P)^2^+1.7493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8969
_reflns_number_total             12634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10234_si_004.cif
_cod_data_source_block           lavallo37_0m_a_sq_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2735.9(13)
_cod_database_code               4133813
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.149
_shelx_estimated_absorpt_t_min   0.120
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C9 = C9-C10 = C11-C10
 1.5 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(B20) \\sim Ueq, Uanis(B4) \\sim Ueq, Uanis(B19) \\sim Ueq, Uanis(B6)
\\sim Ueq, Uanis(B17) \\sim Ueq, Uanis(B15) \\sim Ueq, Uanis(B14) \\sim Ueq,
Uanis(B9) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(B13) \\sim Ueq, Uanis(B2) \\sim
Ueq, Uanis(B7) \\sim Ueq, Uanis(B10) \\sim Ueq, Uanis(B22) \\sim Ueq, Uanis(B3)
\\sim Ueq, Uanis(B8) \\sim Ueq, Uanis(B21) \\sim Ueq, Uanis(B18) \\sim Ueq,
Uanis(B12) \\sim Ueq, Uanis(B11) \\sim Ueq, Uanis(B5) \\sim Ueq, Uanis(B16)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
4.d Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B5(H5A), B6(H6), B10(H10), B12(H12), B13(H13), B14(H14),
 B15(H15), B22(H22)
;
_shelx_res_checksum              82873
_shelx_hkl_checksum              93240
_shelx_fab_checksum              52527
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'