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_4086857
_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 unk
_chemical_formula_moiety         '2(C4 H8 O), C62 H81 Ag2 N4, B F4'
_chemical_formula_sum            'C70 H97 Ag2 B F4 N4 O2'
_chemical_formula_weight         1329.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 99.2266(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.50202(20)
_cell_length_b                   31.8127(5)
_cell_length_c                   17.2528(3)
_cell_measurement_reflns_used    52480
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4800
_cell_measurement_theta_min      1.2790
_cell_volume                     6773.06(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            86841
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         1.650
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of THF and pentane by ---'
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1569
_refine_ls_number_reflns         37836
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0489P)^2^+9.8048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.967
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                32537
_reflns_number_total             37836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00771_si_001.cif
_cod_data_source_block           l2ag2ccphbf4
_cod_depositor_comments
'Adding full bibliography for 4086853--4086857.cif.'
_cod_original_cell_volume        6773.0(2)
_cod_database_code               4086857
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(2) 0.51(2)
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. Restrained distances
 O6S-C7S \\sim O6S-C10S
 with sigma of 0.002
 C8S-C7S \\sim C9S-C8S \\sim C9S-C10S
 with sigma of 0.002
 C4A-C3A \\sim C5A-C4A \\sim C3A-C2A
 with sigma of 0.002
 C5B-C4B \\sim C4B-C3B \\sim C3B-C2B
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(F4B) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F1B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F2B) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(O6S) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C10') \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O6S) = Uanis(O6')
Uanis(C9S) = Uanis(C9')
Uanis(C8S) = Uanis(C8')
Uanis(C10S) = Uanis(C10')
Uanis(C7S) = Uanis(C7')
Uanis(B1A) = Uanis(B1B)
Uanis(F1B) = Uanis(F1A)
Uanis(F3A) = Uanis(F3B)
Uanis(F4B) = Uanis(F4A)
Uanis(F2B) = Uanis(F2A)
Uanis(C2A) = Uanis(C2B)
Uanis(C5A) = Uanis(C4B)
Uanis(C2B) = Uanis(C3A)
Uanis(C5B) = Uanis(C5A)
Uanis(C4A) = Uanis(O1B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4B) = Uanis(C4A)
5. Rigid body (RIGU) restrains
 C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C22, C23, C24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9A, C2AA, C3AA
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C17, C25, C26, C27
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F4A, F2A, B1A, F1A, F3A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 B1A, F4A, F2A, F1A, F3A, F3B, B1B, F1B, F2B, F4B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6S, C9S, H1CA, H2CA, C8S, C10S, C7S, H5CA, H6CA, H7CA, H8CA, H3CA, H4CA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1A, C2A, C5A, H, HA, C3A, C4A, HF, HG, HB, HC, HD, HE
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Same fragment restrains
{O1B, C2B, C3B, C4B, C5B} sigma for 1-2: 0.002, 1-3: 0.002
as
{O1A, C2A, C3A, C4A, C5A}
{F2B, F3B, B1B, F1B, F4B} sigma for 1-2: 0.002, 1-3: 0.002
as
{F4A, F2A, B1A, F1A, F3A}
{C9', C7', O6', C8', C10'} sigma for 1-2: 0.002, 1-3: 0.002
as
{C9S, C7S, O6S, C8S, C10S}
7. Others
 Sof(F2B)=Sof(F3B)=Sof(B1B)=Sof(F1B)=Sof(F4B)=1-FVAR(1)
 Sof(F4A)=Sof(F2A)=Sof(B1A)=Sof(F1A)=Sof(F3A)=FVAR(1)
 Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(O6')=Sof(C8')=
 Sof(H8'A)=Sof(H8'B)=Sof(C10')=Sof(H10A)=Sof(H10B)=1-FVAR(2)
 Sof(C9S)=Sof(H1CA)=Sof(H2CA)=Sof(C7S)=Sof(H3CA)=Sof(H4CA)=Sof(O6S)=Sof(C8S)=
 Sof(H5CA)=Sof(H6CA)=Sof(C10S)=Sof(H7CA)=Sof(H8CA)=FVAR(2)
 Sof(O1B)=Sof(C2B)=Sof(HH)=Sof(HI)=Sof(C3B)=Sof(HJ)=Sof(HK)=Sof(C4B)=Sof(HL)=
 Sof(HM)=Sof(C5B)=Sof(HN)=Sof(HO)=1-FVAR(3)
 Sof(O1A)=Sof(C2A)=Sof(H)=Sof(HA)=Sof(C3A)=Sof(HB)=Sof(HC)=Sof(C4A)=Sof(HD)=
 Sof(HE)=Sof(C5A)=Sof(HF)=Sof(HG)=FVAR(3)
8.a Ternary CH refined with riding coordinates:
 C18(HX), C23(H0BA), C25(H4BA), C16A(H0EA), C19A(H7EA), C23A(H7FA), C25A(H1GA),
  C16B(H4HA), C19B(H1IA), C23B(H1JA), C25B(H5JA), C16C(H6LA), C19C(H3MA),
 C23C(H3NA), C25C(H7NA), C1B(H1RA)
8.b Secondary CH2 refined with riding coordinates:
 C2A(H,HA), C3A(HB,HC), C4A(HD,HE), C5A(HF,HG), C2B(HH,HI), C3B(HJ,HK), C4B(HL,
 HM), C5B(HN,HO), C6(HP,HQ), C7(HR,HS), C9S(H1CA,H2CA), C7S(H3CA,H4CA),
 C8S(H5CA,H6CA), C10S(H7CA,H8CA), C9'(H9'A,H9'B), C7'(H7'A,H7'B), C8'(H8'A,
 H8'B), C10'(H10A,H10B), C2C(H6KA,H7KA), C3C(H8KA,H9KA), C2S(H4OA,H5OA),
 C3S(H6OA,H7OA), C4S(H8OA,H9OA), C5S(H0PA,H1PA), C12S(H2PA,H3PA), C13S(H4PA,
 H5PA), C14S(H6PA,H7PA), C15S(H8PA,H9PA), C0AA(H3QA,H4QA), C1AA(H5QA,H6QA),
 C4AA(H7QA,H8QA), C5AA(H9QA,H0RA)
8.c Me refined with riding coordinates:
 C20A(H8EA,H9EA,H0FA)
8.d Aromatic/amide H refined with riding coordinates:
 C10(HT), C14(HU), C15(HV), C16(HW), C31(H9CA), C32(H0DA), C33(H1DA),
 C34(H2DA), C35(H3DA), C6A(H4DA), C7A(H5DA), C8A(H6DA), C12A(H7DA), C13A(H8DA),
 C14A(H9DA), C6B(H8GA), C7B(H9GA), C8B(H0HA), C12B(H1HA), C13B(H2HA),
 C14B(H3HA), C32B(H2KA), C33B(H3KA), C34B(H4KA), C35B(H5KA), C6C(H0LA),
 C7C(H1LA), C8C(H2LA), C12C(H3LA), C13C(H4LA), C14C(H5LA), C1C(H2RA), C1D(H3RA),
  C31B(H4RA)
8.e Idealised Me refined as rotating group:
 C19(HY,HZ,H0AA), C20(H1AA,H2AA,H3AA), C21(H4AA,H5AA,H6AA), C22(H7AA,H8AA,
 H9AA), C24(H1BA,H2BA,H3BA), C26(H5BA,H6BA,H7BA), C27(H8BA,H9BA,H0CA),
 C17A(H1EA,H2EA,H3EA), C18A(H4EA,H5EA,H6EA), C21A(H1FA,H2FA,H3FA), C22A(H4FA,
 H5FA,H6FA), C24A(H8FA,H9FA,H0GA), C26A(H2GA,H3GA,H4GA), C27A(H5GA,H6GA,H7GA),
 C17B(H5HA,H6HA,H7HA), C18B(H8HA,H9HA,H0IA), C20B(H2IA,H3IA,H4IA), C21B(H5IA,
 H6IA,H7IA), C22B(H8IA,H9IA,H0JA), C24B(H2JA,H3JA,H4JA), C26B(H6JA,H7JA,H8JA),
 C27B(H9JA,H0KA,H1KA), C17C(H7LA,H8LA,H9LA), C18C(H0MA,H1MA,H2MA), C20C(H4MA,
 H5MA,H6MA), C21C(H7MA,H8MA,H9MA), C22C(H0NA,H1NA,H2NA), C24C(H4NA,H5NA,H6NA),
 C26C(H8NA,H9NA,H0OA), C27C(H1OA,H2OA,H3OA), C1A(H0QA,H1QA,H2QA)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'