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_4126501
_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         'Ag C10 Fe2 O10, C32 H12 B F24'
_chemical_formula_sum            'C42 H12 Ag B F24 Fe2 O10'
_chemical_formula_weight         1362.90
_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             2017-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.1650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3046(5)
_cell_length_b                   17.1790(6)
_cell_length_c                   21.7859(9)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      3.00
_cell_volume                     5086.8(3)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33430
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.583
_diffrn_reflns_theta_min         2.997
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0595 before and 0.0482 after correction. The Ratio of minimum to maximum transmission is 0.8943. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7770
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+8.8343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6735
_reflns_number_total             7770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08595_si_002.cif
_cod_data_source_block           rad510a_a_sq
_cod_database_code               4126501
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F8-C20 \\sim F8A-C20 \\sim F7A-C20 \\sim F7-C20 \\sim F9A-C20 \\sim F9-C20
 with sigma of 0.005
 F2-C12 \\sim F2A-C12 \\sim F1A-C12 \\sim F1-C12 \\sim F3-C12 \\sim F3A-C12
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(F8A) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F1A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2A)
\\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.003
Uanis(F3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Rigid body (RIGU) restrains
 F1, F1A, F3, F3A, F2, F2A, F8A, F8, F7A, F7, F9A, F9
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
5. Others
 Sof(F8A)=Sof(F7A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F1A)=Sof(F3A)=Sof(F2A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C15(H15), C17(H17), C19(H19)
;
_shelx_res_checksum              32835
_shelx_hkl_checksum              85462
_shelx_fab_checksum              31744
_olex2_submission_special_instructions 'No special instructions were received'