Fine tuning of intra-lattice electron transfers through site doping in tetraoxolene-bridged iron honeycomb layers.
Sekine, Yoshihiro; Chen, Jian; Eguchi, Naoki; Miyasaka, Hitoshi; Chemical communications (Cambridge, England) 56 (2020) 10867–10870; doi:10.1039/d0cc03808c

data_7127031
_publ_section_title
;
 Fine tuning of intra-lattice electron transfers through site doping in
 tetraoxolene-bridged iron honeycomb layers.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10867
_journal_page_last               10870
_journal_paper_doi               10.1039/d0cc03808c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'Br2.118 C18 Cl3.882 Fe2 O12, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Br2.12 Cl3.88 Fe2 N2 O12'
_chemical_formula_weight         1199.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-28
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:19:11 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.410(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8837(10)
_cell_length_b                   20.7386(13)
_cell_length_c                   12.3417(11)
_cell_measurement_reflns_used    5392
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      30.0470
_cell_measurement_theta_min      1.9260
_cell_volume                     2730.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  70.00   0.50   10.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   10.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0120634000
_diffrn_orient_matrix_UB_12      -0.0241848000
_diffrn_orient_matrix_UB_13      -0.0371304000
_diffrn_orient_matrix_UB_21      0.0451747000
_diffrn_orient_matrix_UB_22      0.0202554000
_diffrn_orient_matrix_UB_23      -0.0169638000
_diffrn_orient_matrix_UB_31      0.0473002000
_diffrn_orient_matrix_UB_32      -0.0131585000
_diffrn_orient_matrix_UB_33      0.0421442000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20720
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.587
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.874
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.1010
_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^)+48.9236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2087
_refine_ls_wR_factor_ref         0.2303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3929
_reflns_number_total             6116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03808c2.cif
_cod_data_source_block           Br-035-d_CCDC-2014804_R1
_cod_depositor_comments
'Adding full bibliography for 7127029--7127048.cif.'
_cod_database_code               7127031
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C42 H56 Cl3.88 Br2.12 Fe2 N2 O12'
_reflns_odcompleteness_completeness 88.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-Br2
 1.88 with sigma of 0.02
 C6-Cl2
 1.73 with sigma of 0.02
 Cl3-C8
 1.73 with sigma of 0.02
3. Rigid bond restraints
 Br1, Br3, Cl3, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Br1 \\sim Br3 \\sim Cl3 \\sim Cl1: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Uanis(Cl2) = Uanis(Br2)
5. Rigid body (RIGU) restrains
 Cl2, Br2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: Br1(0.35834) Cl3(0.65768) Cl2(0.64166) Br3(0.34232) Cl1(0.64166)
 Br2(0.35834)
7.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C10(H10A,H10B), C19(H19A,H19B), C14(H14A,H14B), C13(H13A,
 H13B), C16(H16A,H16B), C11(H11A,H11B), C17(H17A,H17B)
7.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C12(H12A,H12B,
 H12C)
;
_shelx_res_checksum              96457
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.521
_oxdiff_exptl_absorpt_empirical_full_min 0.666