#------------------------------------------------------------------------------
#$Date: 2019-11-26 02:41:52 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242424 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/24/4132441.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_4132441
loop_
_publ_author_name
'DeGayner, Jordan A.'
'Wang, Kunyu'
'Harris, T. David'
_publ_section_title
;
 A Ferric Semiquinoid Single-Chain Magnet via Thermally-Switchable
 Metal-Ligand Electron Transfer.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6550
_journal_page_last               6553
_journal_paper_doi               10.1021/jacs.8b03949
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.5(C12 Cl8 Fe2 O8), 2(C4 H12 N)'
_chemical_formula_sum            'C14 H24 Cl4 Fe N2 O4'
_chemical_formula_weight         482.00
_chemical_name_systematic        (NMe4)2CAFeCl2_100K
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.971(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1004(14)
_cell_length_b                   9.3394(8)
_cell_length_c                   13.8165(13)
_cell_measurement_reflns_used    5440
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.22
_cell_measurement_theta_min      2.79
_cell_volume                     2007.0(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13430
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.590
_diffrn_reflns_theta_min         2.787
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.5790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0817 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.7753. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.092
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0653
_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)+(0.1073P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2891
_reflns_number_total             4166
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b03949_si_001.cif
_cod_data_source_block           nme4fecl2ca_100k
_cod_database_code               4132441
_shelx_shelxl_version_number     2014/7
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Fe1 Fe 0.5000 0.30193(6) 0.7500 0.01818(15) Uani 1 2 d S T P
Cl1 Cl 0.66093(5) 0.31867(9) 0.48713(6) 0.02761(19) Uani 1 1 d . . .
Cl2 Cl 0.40600(5) 0.12617(8) 0.65492(5) 0.02393(17) Uani 1 1 d . . .
O1 O 0.57131(15) 0.3176(2) 0.65137(15) 0.0215(4) Uani 1 1 d . . .
O2 O 0.56615(14) 0.5390(2) 0.34042(15) 0.0216(4) Uani 1 1 d . . .
C1 C 0.53896(18) 0.4021(3) 0.57674(19) 0.0181(5) Uani 1 1 d . . .
C2 C 0.57283(18) 0.4183(3) 0.4941(2) 0.0194(5) Uani 1 1 d . . .
C3 C 0.53728(18) 0.5160(3) 0.4175(2) 0.0186(5) Uani 1 1 d . . .
N1 N 0.66020(18) 0.8447(3) 0.65479(19) 0.0228(5) Uani 1 1 d . . .
C4 C 0.7015(3) 0.8267(4) 0.7631(3) 0.0382(9) Uani 1 1 d . . .
H4A H 0.6779 0.7418 0.7881 0.057 Uiso 1 1 calc GR . .
H4B H 0.6904 0.9115 0.7996 0.057 Uiso 1 1 calc GR . .
H4C H 0.7637 0.8149 0.7733 0.057 Uiso 1 1 calc GR . .
C5 C 0.6812(2) 0.7194(4) 0.5995(3) 0.0302(7) Uani 1 1 d . . .
H5A H 0.7438 0.7111 0.6118 0.045 Uiso 1 1 calc GR . .
H5B H 0.6555 0.7322 0.5276 0.045 Uiso 1 1 calc GR . .
H5C H 0.6584 0.6322 0.6224 0.045 Uiso 1 1 calc GR . .
C6 C 0.6947(4) 0.9768(5) 0.6193(3) 0.0557(14) Uani 1 1 d . . .
H6A H 0.7574 0.9699 0.6334 0.084 Uiso 1 1 calc GR . .
H6B H 0.6793 1.0601 0.6541 0.084 Uiso 1 1 calc GR . .
H6C H 0.6701 0.9874 0.5470 0.084 Uiso 1 1 calc GR . .
C7 C 0.5661(3) 0.8578(6) 0.6353(4) 0.0549(13) Uani 1 1 d . . .
H7A H 0.5408 0.8705 0.5633 0.082 Uiso 1 1 calc GR . .
H7B H 0.5521 0.9409 0.6716 0.082 Uiso 1 1 calc GR . .
H7C H 0.5428 0.7709 0.6582 0.082 Uiso 1 1 calc GR . .
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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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_
_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
Cl2 Fe1 Cl2 92.97(4) . 2_656
O1 Fe1 Cl2 93.97(7) . .
O1 Fe1 Cl2 91.79(6) . 2_656
O1 Fe1 Cl2 93.97(7) 2_656 2_656
O1 Fe1 Cl2 91.79(7) 2_656 .
O1 Fe1 O1 171.63(13) . 2_656
O1 Fe1 O2 93.61(8) . 6_566
O1 Fe1 O2 93.60(8) 2_656 5_666
O1 Fe1 O2 80.30(8) 2_656 6_566
O1 Fe1 O2 80.30(8) . 5_666
O2 Fe1 Cl2 171.60(6) 5_666 2_656
O2 Fe1 Cl2 90.42(7) 5_666 .
O2 Fe1 Cl2 171.60(6) 6_566 .
O2 Fe1 Cl2 90.42(7) 6_566 2_656
O2 Fe1 O2 87.28(13) 6_566 5_666
C1 O1 Fe1 113.76(18) . .
C3 O2 Fe1 112.53(18) . 5_666
O1 C1 C2 123.8(3) . .
O1 C1 C3 116.4(2) . 5_666
C2 C1 C3 119.8(2) . 5_666
C1 C2 Cl1 119.3(2) . .
C1 C2 C3 121.2(3) . .
C3 C2 Cl1 119.5(2) . .
O2 C3 C1 116.4(2) . 5_666
O2 C3 C2 124.7(3) . .
C2 C3 C1 118.9(2) . 5_666
C4 N1 C5 109.2(3) . .
C4 N1 C6 108.6(3) . .
C5 N1 C6 109.2(3) . .
C7 N1 C4 111.5(3) . .
C7 N1 C5 109.4(3) . .
C7 N1 C6 108.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl2 2.3841(8) 2_656
Fe1 Cl2 2.3841(8) .
Fe1 O1 2.001(2) 2_656
Fe1 O1 2.001(2) .
Fe1 O2 2.053(2) 6_566
Fe1 O2 2.053(2) 5_666
Cl1 C2 1.719(3) .
O1 C1 1.296(3) .
O2 Fe1 2.053(2) 5_666
O2 C3 1.286(3) .
C1 C2 1.395(4) .
C1 C3 1.466(4) 5_666
C2 C3 1.403(4) .
C3 C1 1.466(4) 5_666
N1 C4 1.482(4) .
N1 C5 1.484(4) .
N1 C6 1.488(5) .
N1 C7 1.474(5) .
