#------------------------------------------------------------------------------
#$Date: 2021-11-05 01:05:13 +0100 (vie 05 de nov de 2021) $
#$Revision: 270316 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/87/7708714.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7708714
loop_
_publ_author_name
'Reiß, Andreas'
'Donsbach, Carsten'
'Feldmann, Claus'
_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, ω 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/[σ²(Fo²)+(0.0771P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_file
;
TITL Compound_1_a.res in P-1
    compound_1.res
    created by SHELXL-2018/3 at 13:48:04 on 27-Jul-2021
REM Old TITL Compound_1 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.129, Rweak 0.008, Alpha 0.116, Orientation as input
REM Formula found by SHELXT: Fe C4 I2
CELL 0.71073 4.1189 6.2853 7.8308 91.642 92.504 95.757
ZERR 1 0.0026 0.0039 0.0057 0.055 0.056 0.051
LATT 1
SFAC C H Fe I O
UNIT 2 8 1 2 2
DFIX 0.85 0.01 O1 H1
DANG 2.597799 0.02 Fe02 H1
DANG 1.869975 0.02 C004 H1

L.S. 100 0 0
PLAN  2
SIZE 0.01 0.01 0.06
TEMP -60.15
CONF
BOND $H
list 4
MORE -1
fmap 2 53
acta
OMIT 0 50
OMIT 1 -1 2
OMIT -2 6 2
OMIT -1 5 2
OMIT -1 3 0
OMIT 0 2 4
OMIT 3 4 2
REM <olex2.extras>
REM <HklSrc "%.\\Compound_1.hkl">
REM </olex2.extras>

WGHT    0.077100
FVAR       0.89366
I001  4    0.043354    0.727585    0.686269    11.00000    0.03072    0.03412 =
         0.04128   -0.00206   -0.00274    0.00152
FE02  3    0.500000    0.500000    0.500000    10.50000    0.03079    0.02806 =
         0.03611    0.00354   -0.00238    0.00286
O1    5    0.543991    0.745807    0.325741    11.00000    0.05735    0.02787 =
         0.02278    0.00439   -0.00370   -0.00282
H1    2    0.688279    0.850345    0.349797    11.00000   -1.50000
C004  1    0.450917    0.752392    0.149827    11.00000    0.05669    0.07596 =
         0.02632    0.00932   -0.01568   -0.01029
AFIX 137
H00A  2    0.266346    0.646667    0.122780    11.00000   -1.50000
H00B  2    0.632648    0.721368    0.081728    11.00000   -1.50000
H00C  2    0.390023    0.893651    0.124513    11.00000   -1.50000
AFIX   0
HKLF 4




REM  Compound_1_a.res in P-1
REM wR2 = 0.133695, GooF = S = 0.98650, Restrained GooF = 0.98360 for all data
REM R1 = 0.049619 for 372 Fo > 4sig(Fo) and 0.079571 for all 518 data
REM 38 parameters refined using 3 restraints

END

WGHT      0.0772      0.0000

REM Highest difference peak  1.122,  deepest hole -1.155,  1-sigma level  0.310
Q1    1   0.2185  0.7757  0.7743  11.00000  0.05    1.12
Q2    1   0.2167  0.8983  0.5979  11.00000  0.05    1.09
;
_shelx_res_checksum              33625
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I001 I 0.0434(2) 0.72759(19) 0.68627(19) 0.0357(5) Uani 1 1 d . . . . .
Fe02 Fe 0.500000 0.500000 0.500000 0.0317(9) Uani 1 2 d DS . P . .
O1 O 0.544(3) 0.7458(18) 0.3257(18) 0.037(3) Uani 1 1 d D . . . .
H1 H 0.69(2) 0.850(11) 0.350(7) 0.055 Uiso 1 1 d D U . . .
C004 C 0.451(5) 0.752(4) 0.150(3) 0.055(6) Uani 1 1 d D . . . .
H00A H 0.266346 0.646667 0.122780 0.082 Uiso 1 1 calc R U . . .
H00B H 0.632648 0.721368 0.081728 0.082 Uiso 1 1 calc R U . . .
H00C H 0.390023 0.893651 0.124513 0.082 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I001 0.0307(7) 0.0341(7) 0.0413(9) -0.0021(5) -0.0027(4) 0.0015(4)
Fe02 0.0308(17) 0.0281(17) 0.036(3) 0.0035(17) -0.0024(14) 0.0029(14)
O1 0.057(7) 0.028(6) 0.023(9) 0.004(6) -0.004(6) -0.003(6)
C004 0.057(12) 0.076(16) 0.026(16) 0.009(12) -0.016(9) -0.010(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
21 30 -4 0.0977
30 -29 -8 0.0776
-2 19 30 0.0635
-22 21 30 0.0803
-10 -27 30 0.0672
2 -30 -3 0.0979
-1 -1 -15 0.0578
1 14 -30 0.0687
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Fe02 I001 Fe02 91.59(6) 1_455 . ?
I001 Fe02 I001 91.59(6) 1_655 . ?
I001 Fe02 I001 88.41(6) 2_566 . ?
I001 Fe02 I001 180.0 2_566 1_655 ?
I001 Fe02 I001 91.59(6) 2_566 2_666 ?
I001 Fe02 I001 88.41(7) 1_655 2_666 ?
I001 Fe02 I001 180.00(4) . 2_666 ?
O1 Fe02 I001 89.9(4) . . ?
O1 Fe02 I001 86.5(3) 2_666 2_566 ?
O1 Fe02 I001 89.9(4) 2_666 2_666 ?
O1 Fe02 I001 93.5(3) 2_666 1_655 ?
O1 Fe02 I001 93.5(3) . 2_566 ?
O1 Fe02 I001 86.5(3) . 1_655 ?
O1 Fe02 I001 90.1(4) 2_666 . ?
O1 Fe02 I001 90.1(4) . 2_666 ?
O1 Fe02 O1 180.0(6) 2_666 . ?
Fe02 O1 H1 117(2) . . ?
C004 O1 Fe02 132.1(12) . . ?
C004 O1 H1 108(3) . . ?
O1 C004 H00A 109.5 . . ?
O1 C004 H00B 109.5 . . ?
O1 C004 H00C 109.5 . . ?
H00A C004 H00B 109.5 . . ?
H00A C004 H00C 109.5 . . ?
H00B C004 H00C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I001 Fe02 2.852(2) 1_455 ?
I001 Fe02 2.893(2) . ?
Fe02 O1 2.090(13) . ?
Fe02 O1 2.090(13) 2_666 ?
O1 H1 0.852(10) . ?
O1 C004 1.42(3) . ?
C004 H00A 0.9700 . ?
C004 H00B 0.9700 . ?
C004 H00C 0.9700 . ?
