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#$Date: 2019-11-17 10:20:00 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229314 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/66/7046698.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_7046698
loop_
_publ_author_name
'Spiegel, Michael T.'
'Hoogerbrugge, Amanda'
'Truksa, Shamus'
'Smith, Andrew G.'
'Shuford, Kevin L.'
'Klausmeyer, Kevin K.'
'Farmer, Patrick J.'
_publ_section_title
;
 Synthesis of first row transition metal selenomaltol complexes.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9030
_journal_page_last               9037
_journal_paper_doi               10.1039/c8dt01170b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C18 H15 Fe O6 Se3'
_chemical_formula_weight         620.03
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-03-13 deposited with the CCDC.
2018-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.8261(12)
_cell_length_b                   14.8261(12)
_cell_length_c                   16.0571(13)
_cell_measurement_reflns_used    8798
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.75
_cell_volume                     3056.7(4)
_computing_cell_refinement       'Bruker SAINTPLUS'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10165
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.290
_diffrn_reflns_theta_min         2.748
_exptl_absorpt_coefficient_mu    6.130
_exptl_absorpt_correction_T_max  0.347
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_description       block
_exptl_crystal_F_000             1794
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
; 
 Flack x determined using 754 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1651
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0185
_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)+0.4941P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0406
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                1603
_reflns_number_total             1651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01170b2.cif
_cod_data_source_block           pf40
_cod_depositor_comments
'Adding full bibliography for 7046695--7046698.cif.'
_cod_original_cell_volume        3056.7(6)
_cod_database_code               7046698
_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_min   0.377
_shelx_estimated_absorpt_t_max   0.515
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
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
Se1 Se 0.51900(2) 0.21227(2) 0.35952(2) 0.02688(10) Uani 1 1 d . . .
Fe2 Fe 0.6667 0.3333 0.25654(4) 0.01609(14) Uani 1 3 d S T P
O1 O 0.54296(15) 0.30050(15) 0.18675(13) 0.0178(4) Uani 1 1 d . . .
C1 C 0.4466(2) 0.2569(2) 0.21248(19) 0.0184(5) Uani 1 1 d . . .
C2 C 0.4174(2) 0.2160(2) 0.29466(19) 0.0211(6) Uani 1 1 d . . .
C4 C 0.2435(3) 0.1736(3) 0.2643(3) 0.0313(7) Uani 1 1 d . . .
H4 H 0.1737 0.1483 0.2820 0.038 Uiso 1 1 calc R U .
O2 O 0.26882(16) 0.20414(17) 0.18584(17) 0.0290(5) Uani 1 1 d . . .
C6 C 0.3788(3) 0.2677(3) 0.0689(2) 0.0300(7) Uani 1 1 d . . .
H6A H 0.3282 0.2059 0.0381 0.045 Uiso 1 1 calc R U .
H6B H 0.4494 0.2873 0.0508 0.045 Uiso 1 1 calc R U .
H6C H 0.3659 0.3253 0.0579 0.045 Uiso 1 1 calc R U .
C5 C 0.3681(2) 0.2447(2) 0.1587(2) 0.0224(6) Uani 1 1 d . . .
C3 C 0.3135(2) 0.1775(2) 0.3195(2) 0.0274(7) Uani 1 1 d . . .
H3 H 0.2929 0.1543 0.3751 0.033 Uiso 1 1 calc R U .
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'
O O 0.0106 0.0060 '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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 Se1 Fe2 92.20(9) . .
O1 Fe2 O1 91.42(9) 2_655 3_665
O1 Fe2 O1 91.42(9) 2_655 .
O1 Fe2 O1 91.42(9) 3_665 .
O1 Fe2 Se1 80.51(6) 2_655 2_655
O1 Fe2 Se1 107.21(6) 3_665 2_655
O1 Fe2 Se1 159.76(6) . 2_655
O1 Fe2 Se1 159.76(6) 2_655 3_665
O1 Fe2 Se1 80.51(6) 3_665 3_665
O1 Fe2 Se1 107.21(6) . 3_665
Se1 Fe2 Se1 84.18(2) 2_655 3_665
O1 Fe2 Se1 107.21(6) 2_655 .
O1 Fe2 Se1 159.75(6) 3_665 .
O1 Fe2 Se1 80.51(6) . .
Se1 Fe2 Se1 84.18(2) 2_655 .
Se1 Fe2 Se1 84.18(2) 3_665 .
C1 O1 Fe2 126.09(19) . .
O1 C1 C5 120.4(3) . .
O1 C1 C2 121.8(3) . .
C5 C1 C2 117.7(3) . .
C3 C2 C1 118.2(3) . .
C3 C2 Se1 124.7(2) . .
C1 C2 Se1 117.0(2) . .
O2 C4 C3 122.0(3) . .
C4 O2 C5 121.1(3) . .
O2 C5 C1 120.8(3) . .
O2 C5 C6 112.7(3) . .
C1 C5 C6 126.5(3) . .
C4 C3 C2 119.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 C2 1.855(3) .
Se1 Fe2 2.6114(6) .
Fe2 O1 1.991(2) 2_655
Fe2 O1 1.991(2) 3_665
Fe2 O1 1.991(2) .
Fe2 Se1 2.6114(6) 2_655
Fe2 Se1 2.6114(6) 3_665
O1 C1 1.306(3) .
C1 C5 1.386(4) .
C1 C2 1.426(4) .
C2 C3 1.407(4) .
C4 O2 1.328(5) .
C4 C3 1.344(5) .
O2 C5 1.355(4) .
C6 C5 1.471(5) .
