Preparation and Protonation of Fe2(pdt)(CNR)6, Electron-Rich Analogues of Fe2(pdt)(CO)6.
Zhou, Xiaoyuan; Barton, Bryan E.; Chambers, Geoffrey M.; Rauchfuss, Thomas B.; Arrigoni, Federica; Zampella, Giuseppe; Inorganic chemistry 55 (2016) 3401–3412; doi:10.1021/acs.inorgchem.5b02789

data_4347141
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Preparation and Protonation of Fe2(pdt)(CNR)6, Electron-Rich Analogues of
 Fe2(pdt)(CO)6.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3401
_journal_page_last               3412
_journal_paper_doi               10.1021/acs.inorgchem.5b02789
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C45 H30 Cl6 Fe2 N6 S2'
_chemical_formula_sum            'C45 H30 Cl6 Fe2 N6 S2'
_chemical_formula_weight         1043.27
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90.5607(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0929(6)
_cell_length_b                   21.3105(11)
_cell_length_c                   17.7067(9)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.49
_cell_volume                     4562.9(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd54vsa
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            100824
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.431
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.90421
_exptl_absorpt_correction_T_min  0.82754
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_id                cd54vsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-2 -1 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0056(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         8399
_refine_ls_number_restraints     1341
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0662P)^2^+15.2974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7192
_reflns_number_total             8399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02789_si_002.cif
_cod_data_source_block           cd54vsa
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347141
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.868
_shelxl_version_number           2014/6
_shelx_res_checksum              92395
_shelx_hkl_checksum              88685