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_4126498
_publ_section_title
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 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         'F6 Sb, C5 H2 Ag Fe O6'
_chemical_formula_sum            'C5 H2 Ag F6 Fe O6 Sb'
_chemical_formula_weight         557.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.214(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4883(4)
_cell_length_b                   15.1483(10)
_cell_length_c                   13.0405(9)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      3.12
_cell_volume                     1271.56(14)
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11574
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         3.117
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.855
_exptl_absorpt_correction_T_max  0.1561
_exptl_absorpt_correction_T_min  0.1001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0881 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.6413. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.912
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.090
_refine_diff_density_min         -1.523
_refine_diff_density_rms         0.203
_refine_ls_extinction_coef       0.0099(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         2628
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.275
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0222P)^2^+28.9237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2584
_reflns_number_total             2628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08595_si_002.cif
_cod_data_source_block           rad480_0m_a
_cod_database_code               4126498
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.530
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Restrained distances
 Sb2-F11 \\sim Sb1-F2 \\sim Sb2-F7 \\sim Sb1-F1 \\sim Sb2-F12 \\sim Sb1-F4
\\sim Sb1-F3 \\sim Sb2-F9 \\sim Sb2-
 F8 \\sim Sb2-F10 \\sim Sb1-F5 \\sim Sb1-F6
 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
Uanis(F11) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F1) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(Sb2) \\sim Ueq, Uanis(Sb1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Others
 Sof(Sb1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=1-FVAR(1)
 Sof(Sb2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 O6(H6A,H6B)
;
_shelx_res_checksum              96201
_shelx_hkl_checksum              87109
_olex2_submission_special_instructions 'No special instructions were received'