Reversible CO Dissociation of Tricarbonyl Iodide [Fe]-Hydrogenase Models Ligating Acylmethylpyridyl Ligands
Hu, Bowen; Chen, Xiangyang; Gong, Dawei; Cui, Wen; Yang, Xinzheng; Chen, Dafa; Organometallics 35 (2016) 2993–; doi:10.1021/acs.organomet.6b00524

data_4088886
_publ_section_title
;
 Reversible CO Dissociation of Tricarbonyl Iodide [Fe]-Hydrogenase Models
 Ligating Acylmethylpyridyl Ligands
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2993
_journal_paper_doi               10.1021/acs.organomet.6b00524
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C28 H23 Fe I N O4 P'
_chemical_formula_weight         651.19
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.001(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.2032(7)
_cell_length_b                   8.7859(2)
_cell_length_c                   26.7209(7)
_cell_measurement_reflns_used    3333
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8950
_cell_measurement_theta_min      3.3290
_cell_volume                     5199.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11657
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    1.864
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+1.6464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                3501
_reflns_number_total             4583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00524_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4088886