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_4126502
_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         'C12 H30 Ag O3, C32 H12 B F24'
_chemical_formula_sum            'C44 H42 Ag B F24 O3'
_chemical_formula_weight         1193.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.517(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3286(7)
_cell_length_b                   18.3683(10)
_cell_length_c                   22.2169(13)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.91
_cell_volume                     5030.9(5)
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            62884
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.601
_diffrn_reflns_theta_min         2.766
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0732 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.9216.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         15400
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0298P)^2^+7.3382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11830
_reflns_number_total             15400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08595_si_002.cif
_cod_data_source_block           rad397_0m
_cod_database_code               4126502
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.845
_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. Restrained distances
 F22-C44 \\sim F22A-C44 \\sim F23-C44 \\sim F23A-C44 \\sim F24-C44 \\sim
F24A-C44
 with sigma of 0.01
 F9A-C27 \\sim F9-C27 \\sim F8A-C27 \\sim F8-C27 \\sim F7A-C27 \\sim F7-C27
 with sigma of 0.01
3. Rigid bond restraints
 F23, F23A, F24A, F24, F22, F22A
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
 F9A, F9, F8A, F8, F7A, F7
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
4. Uiso/Uaniso restraints and constraints
F23 \\sim F22A \\sim F22 \\sim F24A \\sim F24 \\sim F23A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.01
F9A \\sim F9 \\sim F8A \\sim F8 \\sim F7A \\sim F7: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Sof(F9A)=Sof(F8A)=Sof(F7A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,
 H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C18(H18), C22(H22), C24(H24), C26(H26), C30(H30),
 C32(H32), C34(H34), C38(H38), C40(H40), C42(H42)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              46919
_shelx_hkl_checksum              72921
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'