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_4086853
_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         'C28 H41 Ag N2'
_chemical_formula_sum            'C28 H41 Ag N2'
_chemical_formula_weight         513.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9650(4)
_cell_length_b                   12.6078(3)
_cell_length_c                   19.5211(6)
_cell_measurement_reflns_used    18847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3060
_cell_measurement_theta_min      1.6550
_cell_volume                     2698.69(14)
_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  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -8.76 199.24   1.00   20.00    --   31.76  73.80 -38.21  208
  2  \w     -8.76 199.24   1.00   20.00    --   31.76  73.80  43.29  208
  3  \w     -8.76 199.24   1.00   20.00    --   31.76  73.80 -66.74  208
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'APEX2 Mo source'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0397090000
_diffrn_orient_matrix_UB_12      0.0418251000
_diffrn_orient_matrix_UB_13      0.0096291000
_diffrn_orient_matrix_UB_21      0.0176803000
_diffrn_orient_matrix_UB_22      -0.0064596000
_diffrn_orient_matrix_UB_23      0.0346927000
_diffrn_orient_matrix_UB_31      0.0478763000
_diffrn_orient_matrix_UB_32      0.0371196000
_diffrn_orient_matrix_UB_33      -0.0048210000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32554
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.567
_diffrn_reflns_theta_min         2.087
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.64200
_exptl_absorpt_correction_T_min  0.63435
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of THF and pentane by ---'
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.145
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+2.7813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2980
_reflns_number_total             3796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00771_si_001.cif
_cod_data_source_block           sipragme
_cod_depositor_comments
'Adding full bibliography for 4086853--4086857.cif.'
_cod_original_cell_volume        2698.69(13)
_cod_database_code               4086853
_chemical_oxdiff_formula         C28H41AgN2
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.757
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Fixed Sof: H1B(0.5) H1A(0.5) H1C(0.5)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C8(H8)
3.d Idealised Me refined as rotating group:
 C1(H1B,H1A,H1C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C11(H11A,H11B,H11C)
;
_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_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 2.527
_oxdiff_exptl_absorpt_empirical_full_min 0.716