Design and Characterization of Phosphine Iron Hydrides: Toward Hydrogen-Producing Catalysts.
Weber, Katharina; Weyhermüller, Thomas; Bill, Eckhard; Erdem, Özlen F; Lubitz, Wolfgang; Inorganic chemistry 54 (2015) 6928–6937; doi:10.1021/acs.inorgchem.5b00911

data_4343513
_publ_section_title
;
 Design and Characterization of Phosphine Iron Hydrides: Toward
 Hydrogen-Producing Catalysts.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6928
_journal_page_last               6937
_journal_paper_doi               10.1021/acs.inorgchem.5b00911
_journal_volume                  54
_journal_year                    2015
_chemical_compound_source        tetrahydrofuran,hexane
_chemical_formula_moiety         'C38 H55 Cl Fe N2 P2, 0.5(C4 H8 O)'
_chemical_formula_sum            'C40 H59 Cl Fe N2 O0.5 P2'
_chemical_formula_weight         729.13
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_code                LBZ-WK-510-01
_audit_creation_date             2013-10-16
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                95.545(5)
_cell_angle_beta                 116.869(4)
_cell_angle_gamma                111.468(6)
_cell_formula_units_Z            2
_cell_length_a                   13.1831(10)
_cell_length_b                   13.2434(9)
_cell_length_c                   13.4648(8)
_cell_measurement_reflns_used    45184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.9997
_cell_measurement_theta_min      2.7386
_cell_volume                     1851.8(3)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.996
_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       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41990
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.112
_diffrn_reflns_theta_min         2.934
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.96380
_exptl_absorpt_correction_T_min  0.90976
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         14032
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0387P)^2^+0.7640P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12247
_reflns_number_total             14032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00911_si_002.cif
_cod_data_source_block           8494
_cod_depositor_comments
;Adding full bibliography for 4343511--4343513.cif.

 Adding full bibliography for 4343511--4343513.cif.
;
_cod_original_cell_volume        1851.8(2)
_cod_original_formula_sum        'C40 H59 Cl Fe N2 O0.50 P2'
_cod_database_code               4343513
_shelxl_version_number           2013-2
_shelx_res_checksum              85284
_shelx_hkl_checksum              61899