From an Fe<sub>2</sub>P<sub>3</sub> complex to FeP nanoparticles as efficient electrocatalysts for water-splitting.
Yao, Shenglai; Forstner, Viktoria; Menezes, Prashanth W.; Panda, Chakadola; Mebs, Stefan; Zolnhofer, Eva M.; Miehlich, Matthias E.; Szilvási, Tibor; Ashok Kumar, Nanjundan; Haumann, Michael; Meyer, Karsten; Grützmacher, Hansjörg; Driess, Matthias; Chemical science 9 (2018) 8590–8597; doi:10.1039/c8sc03407a

data_1549961
_publ_section_title
;
 From an Fe<sub>2</sub>P<sub>3</sub> complex to FeP nanoparticles as
 efficient electrocatalysts for water-splitting.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              8590
_journal_page_last               8597
_journal_paper_doi               10.1039/c8sc03407a
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety
'2(C54 H74 Fe2 N4 P3), 2(C24 H48 K O6), 2(C4 O)'
_chemical_formula_sum            'C164 H244 Fe4 K2 N8 O14 P6'
_chemical_formula_weight         3039.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-08-28 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.729(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.0839(4)
_cell_length_b                   18.8962(3)
_cell_length_c                   13.6307(2)
_cell_measurement_reflns_used    4604
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3180
_cell_measurement_theta_min      3.5640
_cell_volume                     4196.05(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8670
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.370
_diffrn_reflns_theta_min         3.582
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28403
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4248
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1464P)^2^+8.9840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3777
_reflns_number_total             4248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03407a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1549960--1549961.cif.'
_cod_original_cell_volume        4196.05(14)
_cod_database_code               1549961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C00N-C0AA \\sim C0AA-C1AA \\sim C1AA-C5
 with sigma of 0.02
 C00Q-O00K \\sim C00Q-O1
 with sigma of 0.02
3. Others
 Fixed Sof: P003(0.25) P004(0.5) O00K(0.3) C00N(0.5) H00A(0.5) H00B(0.5)
 O00P(0.5) K3(0.25) C1AA(0.5) H1AA(0.5) H1AB(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) O2(0.25) O1(0.2)
4.a Ternary CH refined with riding coordinates:
 C00D(H00L), C00E(H00M)
4.b Secondary CH2 refined with riding coordinates:
 C00N(H00A,H00B), C00O(H00C,H00D), C00Q(H00E,H00F), C00R(H00G,H00H), C1AA(H1AA,
 H1AB), C0AA(H0AA,H0AB), C5(H5A,H5B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00I), C00B(H00J), C00C(H00K), C00F(H00N)
4.d Idealised Me refined as rotating group:
 C00G(H00O,H00P,H00Q), C00H(H00R,H00S,H00T), C00I(H00U,H00V,H00W), C00J(H00X,
 H00Y,H)
;
_shelx_res_checksum              53433
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'