A dinuclear silver hydride and an umpolung reaction of CO2
Tate, Brandon K.; Wyss, Chelsea M.; Bacsa, John; Kluge, Kelly; Gelbaum, Leslie; Sadighi, Joseph P.; Chemical Science 4 (2013) 3068–; doi:10.1039/c3sc50896j

data_1514769
_publ_section_title
;
 A dinuclear silver hydride and an umpolung reaction of CO2
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              3068
_journal_paper_doi               10.1039/c3sc50896j
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety
'(C27 H76 N2)2 Ag2, (C H9 O), C F3 O3 S, 2(C4 H8 O)'
_chemical_formula_sum            'C67 H101 Ag2 F3 N4 O6 S'
_chemical_formula_weight         1363.33
_chemical_name_systematic
;
?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-03-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled Mar 21 2013 11:17:50, GUI svn.r4438)
;
_cell_angle_alpha                74.8830(10)
_cell_angle_beta                 79.9550(10)
_cell_angle_gamma                76.1030(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5882(11)
_cell_length_b                   16.8592(17)
_cell_length_c                   20.800(2)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.980
_cell_measurement_theta_min      2.348
_cell_volume                     3454.7(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            53022
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.105
_diffrn_reflns_theta_min         1.810
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7507
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0525 before and 0.0429 after correction.
The Ratio of minimum to maximum transmission is 0.7507.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.678
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.173
_refine_diff_density_max         1.741
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         23653
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+1.2083P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15943
_reflns_number_total             23653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3sc50896j.txt
_cod_data_source_block           sipr2ag2
_cod_database_code               1514769
_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
C7S-C6S = C8S-C7S = C9S-C8S
1.52 with sigma of 0.02
C7S'-C6S' = C8S'-C7S' = C9S'-C8S'
1.52 with sigma of 0.01
O2S'-C9S' = O2S'-C6S'
1.442 with sigma of 0.02
O2S'-C6S' = O2S'-C9S' = O2S-C9S = O2S-C6S
1.442 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2S) = Uanis(O2S')
4. Others
Sof(O2S)=Sof(C6S)=Sof(C7S)=Sof(C8S)=Sof(C9S)=1-Sof(C6S)=1-Sof(C6S)=1-Sof(C6S)=
1-Sof(C6S)=1-Sof(C6S)
5.a Ternary CH refined with riding coordinates:
C4(H4), C11(H11), C18(H18), C25(H25), C35(H35), C42(H42), C49(H49), C56(H56)
5.b Secondary CH2 refined with riding coordinates:
C14(H14A,H14B), C15(H15A,H15B), C45(H45A,H45B), C46(H46A,H46B), C2S(H2SA,
H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB)
5.c Aromatic/amide H refined with riding coordinates:
C7(H7), C8(H8), C9(H9), C21(H21), C22(H22), C23(H23), C38(H38), C39(H39),
C52(H52), C53(H53), C54(H54), C40(H40)
5.d Idealised Me refined as rotating group:
C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C36(H36A,
H36B,H36C), C37(H37A,H37B,H37C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C57(H57A,H57B,H57C), C58(H58A,H58B,
H58C)
;
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.665
_shelxl_version_number           2012-9