Stable Mono- and Dinuclear Organosilver Complexes
Tate, Brandon K.; Jordan, Abraham J.; Bacsa, John; Sadighi, Joseph P.; Organometallics 36 (2016) 964–; doi:10.1021/acs.organomet.6b00771

data_4086854
_publ_section_title
;
 Stable Mono- and Dinuclear Organosilver Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              964
_journal_paper_doi               10.1021/acs.organomet.6b00771
_journal_volume                  36
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C56 H81 Ag2 N4), 2(B F4)'
_chemical_formula_sum            'C112 H162 Ag4 B2 F8 N8'
_chemical_formula_weight         2225.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-22
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.219(4)
_cell_angle_gamma                90
_cell_formula_units_Z            3
_cell_length_a                   24.156(7)
_cell_length_b                   12.240(4)
_cell_length_c                   29.519(9)
_cell_measurement_reflns_used    9368
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.964
_cell_measurement_theta_min      2.482
_cell_volume                     8460(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            52391
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.572
_diffrn_reflns_theta_min         1.710
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0690 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.7657.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       prism
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.808
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.372
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.055(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         23570
_refine_ls_number_restraints     590
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0500P)^2^+6.8790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                22116
_reflns_number_total             23570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00771_si_001.cif
_cod_data_source_block           sidippag2muet
_cod_depositor_comments
'Adding full bibliography for 4086853--4086857.cif.'
_cod_database_code               4086854
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.945(16) 0.055(16)
2. 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
3. Shared sites
{C2B, C2A}
{C1A, C1B}
4. Restrained distances
 Ag2-H1BB = Ag1-H1BA
 2.44 with sigma of 0.02
 H1BA-C1B = C1B-H1BB
 0.999 with sigma of 0.02
 Ag3B-H30C
 2.44 with sigma of 0.02
 H30C-Ag3B
 2.44 with sigma of 0.02
 H30D-C31B
 2.07 with sigma of 0.01
 H30C-C30B = C30B-H30D
 0.999 with sigma of 0.02
 C31B-H30C
 2.07 with sigma of 0.01
 C2A-H1BB
 2.05 with sigma of 0.02
 H1BA-C2A
 2.07 with sigma of 0.02
 H30A-C30A = C30A-H30B
 0.999 with sigma of 0.02
 H30A-C31A
 2.07 with sigma of 0.01
 H30B-C31A
 2.07 with sigma of 0.01
 Ag4-H30B
 2.44 with sigma of 0.02
 H30A-Ag3
 2.44 with sigma of 0.02
 H30C-H30D
 1.632 with sigma of 0.04
 H1BA-H1BB
 1.632 with sigma of 0.04
 H30A-H30B
 1.632 with sigma of 0.04
 Ag3B-H30C \\sim Ag4B-H30D
 with sigma of 0.005
 Ag3B-C58 \\sim Ag3-C58
 with sigma of 0.01
 Ag4B-C32 \\sim Ag4-C32
 with sigma of 0.01
 Ag3-H30A \\sim Ag4-H30B
 with sigma of 0.005
 Ag3B-C30B \\sim Ag3-C30A
 with sigma of 0.01
 Ag4B-C30B \\sim Ag4-C30A
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
Ag4B: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C30A \\sim Ag3B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(Ag4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.006
Uanis(Ag3B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.008
Uanis(Ag3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Ag4B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C30A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.01
: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C31A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Ag1) = Uanis(Ag2)
Uanis(C1A) = Uanis(C1B)
Uanis(Ag3B) = Uanis(Ag3)
Uanis(Ag4B) = Uanis(Ag4)
Uanis(C2B) = Uanis(C2A)
Uanis(C30B) = Uanis(C30A)
Uanis(C31B) = Uanis(C31A)
6. Rigid body (RIGU) restrains
 C59, C64, C69, C63, C65, C66, C67
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C30A, C31A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C32, C33, C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46,
  C47, C48, C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61,
 C62, C63, C64, C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77,
  C78, C79, C80, C81, C82, C83, C84, C30A, C31A, C30B, C31B, C0AA, C3, C5, C6,
 C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22,
 C23, C24, C25, C26, C27, C28, C29, C1B, C2B, C1A, C2A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7. Same fragment restrains
{Ag3B, Ag4B} sigma for 1-2: 0.002, 1-3: 0.002
as
{Ag3, Ag4}
8. Others
 Sof(Ag2)=1-FVAR(1)
 Sof(C1B)=Sof(C2B)=0.5*(1-FVAR(2))
 Sof(C1A)=Sof(C2A)=0.5*FVAR(2)
 Sof(Ag1)=FVAR(1)
 Fixed Sof: Ag3(0.5) Ag4(0.5) C30A(0.5) C31A(0.5) H31A(0.5) H31B(0.5)
 H31C(0.5) Ag3B(0.5) Ag4B(0.5) C30B(0.5) C31B(0.5) H31D(0.5) H31E(0.5)
 H31F(0.5) H1BA(0.5) H1BB(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) H30C(0.5)
 H30D(0.5) H30A(0.5) H30B(0.5)
9.a Ternary CH refined with riding coordinates:
 C38(H38), C41(H41), C52(H52), C55(H55), C65(H65), C68(H68), C79(H79),
 C82(H82), C10(H10), C13(H13), C24(H24), C27(H27)
9.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B), C71(H71A,H71B), C72(H72A,H72B), C16(H16A,
 H16B), C17(H17A,H17B)
9.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C35(H35), C36(H36), C48(H48), C49(H49), C50(H50), C61(H61),
 C62(H62), C63(H63), C75(H75), C76(H76), C77(H77), C6(H6), C7(H7), C8(H8),
 C20(H20), C21(H21), C22(H22)
9.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C),
 C70(H70A,H70B,H70C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C2A(H2AA,H2AB,H2AC)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id SIDippAg2muEt
_olex2_submission_special_instructions 'No special instructions were received'