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_4126503
_publ_section_title
;
 Heterobimetallic Silver--Iron Complexes Involving Fe(CO)5 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08595
_journal_year                    2017
_chemical_formula_moiety         'C54 H66 Ag P2, C32 H12 B F24'
_chemical_formula_sum            'C86 H78 Ag B F24 P2'
_chemical_formula_weight         1748.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7661(8)
_cell_length_b                   9.2289(3)
_cell_length_c                   34.1516(12)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      3.01
_cell_volume                     7776.2(4)
_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      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            26396
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.490
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0727 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.8993. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         8022
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0397P)^2^+18.9150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6573
_reflns_number_total             8022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08595_si_002.cif
_cod_data_source_block           rad509_0m_a
_cod_database_code               4126503
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.931
_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
 F6-C35 \\sim F9-C35 \\sim F4-C35 \\sim F7-C35 \\sim F5-C35 \\sim F8-C35
 with sigma of 0.01
 F14-C43 \\sim F17-C43 \\sim F15-C43 \\sim F18-C43 \\sim F13-C43 \\sim F16-C43
 with sigma of 0.02
 F4-F5 \\sim F4-F6 \\sim F5-F6 \\sim F7-F8 \\sim F7-F9 \\sim F8-F9
 with sigma of 0.04
 C35-F4 \\sim C35-F5 \\sim C35-F6 \\sim C35-F7 \\sim C35-F8 \\sim C35-F9 \\sim
C35-C32
 with sigma of 0.02
 F16-F17 \\sim F16-F18 \\sim F17-F18 \\sim F13-F14 \\sim F13-F15
 with sigma of 0.04
 C43-F16 \\sim C43-F17 \\sim C43-F18 \\sim C43-F13 \\sim C43-F14 \\sim C43-F15
\\sim C43-C40
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(F7) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F9) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.005
Uanis(F16) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F14) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 F4, F5, F6, F7, F8, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16, F17, F18, F13, F14, F15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F7)=Sof(F8)=Sof(F9)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=1-FVAR(2)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23), C29(H29), C31(H31),
 C33(H33), C37(H37), C39(H39), C41(H41)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              23450
_shelx_hkl_checksum              24200
_olex2_submission_special_instructions 'No special instructions were received'