Heterobimetallic Silver‒Iron Complexes Involving Fe(CO)5 Ligands
Wang, Guocang; Ceylan, Yavuz S.; Cundari, Thomas R.; Dias, H. V. Rasika; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08595

data_4126500
_publ_section_title
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 Heterobimetallic Silver--Iron Complexes Involving Fe(CO)5 Ligands
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_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08595
_journal_year                    2017
_chemical_formula_moiety         'C17 H12 Ag Fe N2 O5, C32 H12 B F24'
_chemical_formula_sum            'C49 H24 Ag B F24 Fe N2 O5'
_chemical_formula_weight         1351.23
_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             2017-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                80.6420(10)
_cell_angle_beta                 75.0590(10)
_cell_angle_gamma                84.1060(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6321(4)
_cell_length_b                   14.4148(5)
_cell_length_c                   14.8557(5)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      2.87
_cell_volume                     2573.58(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.96
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker D8 Quest with a Photon 100 CMOS detector'
_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  0.0204
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25272
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.870
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0557 before and 0.0445 after correction. The Ratio of minimum to maximum transmission is 0.8278. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         10633
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0410P)^2^+3.4954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9302
_reflns_number_total             10633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08595_si_002.cif
_cod_data_source_block           rad531_0m_a
_cod_database_code               4126500
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.757
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F19-F20 \\sim F19-F21 \\sim F20-F21 \\sim F21A-F19A \\sim F21A-F20A \\sim
F19A-F20A
 with sigma of 0.008
 C48-F19 \\sim C48-F20 \\sim C48-F21 \\sim C48-C44 \\sim C48-F21A \\sim
C48-F19A \\sim C48-F20A
 with sigma of 0.02
 F16-F17 \\sim F16-F18 \\sim F17-F18 \\sim F18A-F17A \\sim F18A-F16A \\sim
F17A-F16A
 with sigma of 0.04
 C41-F16 \\sim C41-F17 \\sim C41-F18 \\sim C41-C38 \\sim C41-F18A \\sim
C41-F17A \\sim C41-F16A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F19) \\sim Ueq, Uanis(F19A) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F21A)
\\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F20A) \\sim Ueq: with sigma of 0.008 and
sigma for terminal atoms of 0.008
Uanis(F18A) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F16A) \\sim Ueq, Uanis(F17)
\\sim Ueq, Uanis(F17A) \\sim Ueq, Uanis(F18) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 F16, F17, F18, F19, F20, F21, C38, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16, F17, F18, C38, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19, F20, F21, C44, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19A, F20A, F21A, C44, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16A, F17A, F18A, C38, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(2)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15), C19(H19), C21(H21),
 C23(H23), C27(H27), C29(H29), C31(H31), C35(H35), C37(H37), C39(H39), C43(H43),
  C45(H45), C47(H47)
6.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
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_shelx_res_checksum              75630
_shelx_hkl_checksum              54961
_olex2_submission_special_instructions 'No special instructions were received'