Effects of Catalyst Phase on the Hydrogen Evolution Reaction of Water Splitting: Preparation of Phase-Pure Films of FeP, Fe2P, and Fe3P and Their Relative Catalytic Activities
Schipper, Desmond E.; Zhao, Zhenhuan; Thirumalai, Hari; Leitner, Andrew P.; Donaldson, Samantha L.; Kumar, Arvind; Qin, Fan; Wang, Zhiming; Grabow, Lars C.; Bao, Jiming; Whitmire, Kenton H.; Chemistry of Materials 30 (2018) 3588–; doi:10.1021/acs.chemmater.8b01624

data_4003097
_publ_section_title
;
 Effects of Catalyst Phase on the Hydrogen Evolution Reaction of Water
 Splitting: Preparation of Phase-Pure Films of FeP, Fe2P, and Fe3P and
 Their Relative Catalytic Activities
;
_journal_issue                   10
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3588
_journal_paper_doi               10.1021/acs.chemmater.8b01624
_journal_volume                  30
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H20 Fe2 O8 P2'
_chemical_formula_sum            'C16 H20 Fe2 O8 P2'
_chemical_formula_weight         513.96
_chemical_name_systematic
(\m~2~-di-tert-butyldiphosphine-P,P\')-octacarbonyl-di-iron
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2458(2)
_cell_length_b                   10.2458(2)
_cell_length_c                   21.1573(7)
_cell_measurement_reflns_used    17163
_cell_measurement_temperature    173
_cell_measurement_theta_max      31.7170
_cell_measurement_theta_min      1.9280
_cell_volume                     2221.02(10)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
;
SCXMini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38368
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.698
_diffrn_reflns_theta_min         2.209
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1052.1658
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0367P)^2^+0.9026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.690
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3461
_reflns_number_total             3706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b01624_si_002.cif
_cod_data_source_block           Compound3
_cod_original_cell_volume        2221.03(13)
_cod_database_code               4003097
_shelx_shelxl_version_number     2017/1
_oxdiff_exptl_absorpt_empirical_full_min 0.900
_oxdiff_exptl_absorpt_empirical_full_max 1.101
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              75346
_shelx_hkl_checksum              52219