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_7127035
_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
'0.5(Br0.96 C36 Cl11.04 Fe4 O24), 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Br0.48 Cl5.52 Fe2 N2 O12'
_chemical_formula_weight         1126.63
_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
_audit_creation_date             2020-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-04 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.308(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7693(7)
_cell_length_b                   20.6834(12)
_cell_length_c                   12.2409(8)
_cell_measurement_reflns_used    4654
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.1930
_cell_measurement_theta_min      1.9590
_cell_volume                     2673.7(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.885
_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   30.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   30.00    --  -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      0.0570106000
_diffrn_orient_matrix_UB_12      -0.0070019000
_diffrn_orient_matrix_UB_13      -0.0183653000
_diffrn_orient_matrix_UB_21      -0.0285033000
_diffrn_orient_matrix_UB_22      0.0098059000
_diffrn_orient_matrix_UB_23      -0.0546885000
_diffrn_orient_matrix_UB_31      0.0211468000
_diffrn_orient_matrix_UB_32      0.0321321000
_diffrn_orient_matrix_UB_33      0.0126884000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.1135
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22556
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.113
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78439
_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    1.399
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1161
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.919
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         7609
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.2150
_refine_ls_R_factor_gt           0.1294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+49.4766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2567
_refine_ls_wR_factor_ref         0.3004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3951
_reflns_number_total             7609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03808c2.cif
_cod_data_source_block           Br-010-d_CCDC-2014805_R1
_cod_depositor_comments
'Adding full bibliography for 7127029--7127048.cif.'
_cod_database_code               7127035
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H56 Cl5.4 Br0.6 Fe2 N2 O12'
_reflns_odcompleteness_completeness 88.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.04
_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
 Cl2-C9 \\sim Cl3-C3 \\sim Cl1-C6
 with sigma of 0.02
 Br1-C6 \\sim Br2-C9 \\sim Br3-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim C9 \\sim Br2: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Cl1 \\sim C6 \\sim Br1: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Cl3 \\sim Br3 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
4. Rigid body (RIGU) restrains
 Cl2, C9, Br2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, C6, Br1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3, C3, Br3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Br1)=Sof(Br2)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl1)=FVAR(1)
 Sof(Br3)=1-FVAR(2)
 Sof(Cl3)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C7(H7A,H7B), C14(H14A,H14B), C10(H10A,H10B), C13(H13A,H13B),
 C16(H16A,H16B), C11(H11A,H11B), C12(H12A,H12B)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C1A(H1AA,H1AB,
 H1AC)
;
_shelx_res_checksum              2317
_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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.703