Protonation and Electrochemical Properties of Bisphosphide Diiron Hexacarbonyl Complex Bearing Amino Groups on the Bridge
Shimamura, Takehiko; Maeno, Yuki; Kubo, Kazuyuki; Kume, Shoko; Greco, Claudio; Mizuta, Tsutomu; Dalton Transactions  (2019) –; doi:10.1039/C9DT03427G

data_7701356
_publ_section_title
;
 Protonation and Electrochemical Properties of Bisphosphide Diiron
 Hexacarbonyl Complex Bearing Amino Groups on the Bridge
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03427G
_journal_year                    2019
_chemical_formula_sum            'C24 H26 Fe2 N2 O6 P2'
_chemical_formula_weight         612.11
_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
_audit_update_record
;
2019-08-22 deposited with the CCDC.    2019-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.151(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.352(3)
_cell_length_b                   12.479(3)
_cell_length_c                   17.703(4)
_cell_measurement_reflns_used    1408
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.9233
_cell_measurement_theta_min      2.3809
_cell_volume                     2607.4(11)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2(Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1(Bruker AXS)'
_computing_publication_material  'Generate Report (Bruker AXS)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15432
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.79
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.0267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                5526
_reflns_number_total             6180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03427g2.cif
_cod_data_source_block           I
_cod_original_cell_volume        2607.4(9)
_cod_database_code               7701356
_shelx_res_checksum              71495