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_7708714
_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         'C2 H8 Fe I2 O2'
_chemical_formula_sum            'C2 H8 Fe I2 O2'
_chemical_formula_weight         373.73
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                91.64(6)
_cell_angle_beta                 92.50(6)
_cell_angle_gamma                95.76(5)
_cell_formula_units_Z            1
_cell_length_a                   4.119(3)
_cell_length_b                   6.285(4)
_cell_length_c                   7.831(6)
_cell_measurement_reflns_used    1502
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.60
_cell_volume                     201.4(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area LANA 1.71.6.0 (STOE, 2017)
;
_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      213.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.729
_diffrn_measured_fraction_theta_max 0.729
_diffrn_measurement_details
;
 271 frames, detector distance = 100 mm
;
_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  0.0980
_diffrn_reflns_av_unetI/netI     0.1151
_diffrn_reflns_Laue_measured_fraction_full 0.729
_diffrn_reflns_Laue_measured_fraction_max 0.729
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1122
_diffrn_reflns_point_group_measured_fraction_full 0.729
_diffrn_reflns_point_group_measured_fraction_max 0.729
_diffrn_reflns_theta_full        24.986
_diffrn_reflns_theta_max         24.986
_diffrn_reflns_theta_min         3.259
_exptl_absorpt_coefficient_mu    9.455
_exptl_absorpt_correction_T_max  0.4155
_exptl_absorpt_correction_T_min  0.2483
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             168
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.122
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         518
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0771P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                372
_reflns_number_total             518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02523f2.cif
_cod_data_source_block           compound_1
_cod_database_code               7708714
_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   0.911
_shelx_estimated_absorpt_t_min   0.601
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 Fe02-H1
 2.597799 with sigma of 0.02
 C004-H1
 1.869975 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C004(H00A,H00B,H00C)
;
_shelx_res_checksum              33625
_olex2_submission_special_instructions 'No special instructions were received'