Insights into the naphthalenide-driven synthesis and reactivity of zerovalent iron nanoparticles
Reiß, Andreas; Donsbach, Carsten; Feldmann, Claus; Dalton Transactions  (2021) –; doi:10.1039/D1DT02523F

data_7708715
_publ_section_title
;
 Insights into the naphthalenide-driven synthesis and reactivity of
 zerovalent iron nanoparticles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02523F
_journal_year                    2021
_chemical_formula_moiety
'C18 H15 Fe1 I3 P1, C19 H18 P1, 0.25(C18 H15 P1), 1.5(C7 H8)'
_chemical_formula_sum            'C52 H48.75 Fe I3 P2.25'
_chemical_formula_weight         1179.89
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            8
_cell_length_a                   15.8388(8)
_cell_length_b                   15.8388(8)
_cell_length_c                   46.513(4)
_cell_measurement_reflns_used    7980
_cell_measurement_temperature    213.15
_cell_measurement_theta_max      23.47
_cell_measurement_theta_min      1.425
_cell_volume                     10105.3(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      213.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.1233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            20673
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.485
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.6293
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area X-Red32 1.63.4.0 (STOE, 2017)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       plate
_exptl_crystal_F_000             4636
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.53(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.714
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11403
_refine_ls_number_restraints     367
_refine_ls_restrained_S_all      0.706
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.918
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                4865
_reflns_number_total             11403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02523f2.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        10105.3(13)
_cod_database_code               7708715
_shelx_shelxl_version_number     2018/3
_audit_contact_author
;
      Prof. Dr. Claus Feldmann
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.535
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.47(3)
 0.53(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C53 \\sim C58 \\sim C57 \\sim C56 \\sim C55 \\sim C54: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C66 \\sim C71 \\sim C70 \\sim C69 \\sim C68 \\sim C67: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C65 \\sim C59 \\sim C64 \\sim C63 \\sim C62 \\sim C60 \\sim C61: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C53A \\sim C58A \\sim C57A \\sim C56A \\sim C55A \\sim C54A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C53) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C66) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C53A) \\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(C57A) \\sim Ueq,
Uanis(C56A) \\sim Ueq, Uanis(C55A) \\sim Ueq, Uanis(C54A) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C53, C58, C57, C56, C55, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C66, C71, C70, C69, C68, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53A, C58A, C57A, C56A, C55A, C54A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C54A)=Sof(H54A)=Sof(C53A)=Sof(C58A)=Sof(H58A)=Sof(C57A)=Sof(H57A)=
 Sof(C56A)=Sof(H56A)=Sof(C55A)=Sof(H55A)=1-FVAR(1)
 Sof(C53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=
 Sof(H57)=Sof(C58)=Sof(H58)=FVAR(1)
 Fixed Sof: H52A(0.33333) H52B(0.33333) H52C(0.33333) H31A(0.33333)
 H31B(0.33333) H31C(0.33333) H38A(0.33333) H38B(0.33333) H38C(0.33333)
 H45A(0.33333) H45B(0.33333) H45C(0.33333)
6.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C26(H26), C24(H24), C37(H37), C15(H15), C27(H27), C20(H20),
 C42(H42), C47(H47), C28(H28), C40(H40), C12(H12), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C30(H30), C33(H33), C67(H67), C6(H6), C68(H68), C4(H4),
 C2(H2), C3(H3), C64(H64), C60(H60), C61(H61), C62(H62), C63(H63), C43(H43),
 C17(H17), C21(H21), C36(H36), C8(H8), C29(H29), C18(H18), C70(H70), C41(H41),
 C10(H10), C71(H71), C11(H11), C69(H69), C48(H48), C49(H49), C50(H50), C51(H51),
  C5(H5), C34(H34), C9(H9), C23(H23), C35(H35), C22(H22), C44(H44), C16(H16),
 C54A(H54A), C58A(H58A), C57A(H57A), C56A(H56A), C55A(H55A)
6.b Fitted hexagon refined as free rotating group:
 C53(C54,C55,C56,C57,C58), C64(C59,C60,C61,C62,C63), C54A(C53A,C58A,C57A,C56A,
 C55A)
6.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C31(H31A,H31B,H31C), C65(H65A,H65B,H65C), C72(H72A,H72B,
 H72C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              68856
_olex2_submission_special_instructions 'No special instructions were received'