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_4086856
_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_formula_moiety         '2(C4 H8 O), C60 H81 Ag2 N4, B F4'
_chemical_formula_sum            'C68 H97 Ag2 B F4 N4 O2'
_chemical_formula_weight         1305.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                86.8617(10)
_cell_angle_beta                 79.8545(10)
_cell_angle_gamma                88.8799(9)
_cell_formula_units_Z            2
_cell_length_a                   10.22449(11)
_cell_length_b                   16.3504(2)
_cell_length_c                   20.3736(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                     3347.49(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'APEX2 v2014.11 (Bruker, 2014)'
_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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker D8 diffractometer with APEX2 detector'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            68935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         2.024
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_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    1.295
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         18720
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0605P)^2^+3.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15344
_reflns_number_total             18720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00771_si_001.cif
_cod_data_source_block           a233_0m_[ag2ph]+
_cod_depositor_comments
'Adding full bibliography for 4086853--4086857.cif.'
_cod_original_cell_volume        3347.50(7)
_cod_database_code               4086856
_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
 C3S-C4S \\sim C5S-C4S \\sim C3S-C2S
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C2S') \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C2S) \\sim Ueq, Uanis(C4S') \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C4S) = Uanis(O1S')
Uanis(C2S') = Uanis(C5S)
4. Rigid body (RIGU) restrains
 O1S, C2S, H2SC, H2SD, C3S, H3SC, H3SD, C4S, C5S, H5SC, H5SD
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1S', C2S', H2SA, H2SB, C3S', C4S', H4SA, H4SB, C5S', H5SA, H5SB
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{O1S', C2S', C3S', C4S', C5S'} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1S, C2S, C3S, C4S, C5S}
6. Others
 Fixed Sof: O1S'(0.5) C2S'(0.5) H2SA(0.5) H2SB(0.5) C3S'(0.5) H3SA(0.5)
 H3SB(0.5) C4S'(0.5) H4SA(0.5) H4SB(0.5) C5S'(0.5) H5SA(0.5) H5SB(0.5) O1S(0.5)
 C2S(0.5) H2SC(0.5) H2SD(0.5) C3S(0.5) H3SC(0.5) H3SD(0.5) C4S(0.5) H4SC(0.5)
 H4SD(0.5) C5S(0.5) H5SC(0.5) H5SD(0.5)
7.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C28(H28), C31(H31), C41(H41), C44(H44), C55(H55), C58(H58)
7.b Secondary CH2 refined with riding coordinates:
 C2S'(H2SA,H2SB), C3S'(H3SA,H3SB), C4S'(H4SA,H4SB), C5S'(H5SA,H5SB), C2S(H2SC,
 H2SD), C3S(H3SC,H3SD), C4S(H4SC,H4SD), C5S(H5SC,H5SD), C20(H20A,H20B),
 C21(H21A,H21B), C47(H47A,H47B), C48(H48A,H48B), C7S(H7SA,H7SB), C8S(H8SA,H8SB),
  C9S(H9SA,H9SB), C10S(H10A,H10B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C2(H2),
 C24(H24), C25(H25), C26(H26), C37(H37), C38(H38), C39(H39), C51(H51), C52(H52),
  C53(H53)
7.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C)
;
_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 '[Ag2Ph]+'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.832
_oxdiff_exptl_absorpt_empirical_full_min 0.371