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_7127036
_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
'Br0.6 C18 Cl5.4 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Br0.6 Cl5.4 Fe2 N2 O15'
_chemical_formula_weight         1266.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-07-31
_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                 108.080(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2076(7)
_cell_length_b                   21.8087(7)
_cell_length_c                   14.3967(5)
_cell_measurement_reflns_used    15682
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.4930
_cell_measurement_theta_min      1.7470
_cell_volume                     6031.4(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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      -0.0215527000
_diffrn_orient_matrix_UB_12      -0.0191622000
_diffrn_orient_matrix_UB_13      0.0181457000
_diffrn_orient_matrix_UB_21      0.0298298000
_diffrn_orient_matrix_UB_22      -0.0114946000
_diffrn_orient_matrix_UB_23      0.0362312000
_diffrn_orient_matrix_UB_31      -0.0029846000
_diffrn_orient_matrix_UB_32      0.0236382000
_diffrn_orient_matrix_UB_33      0.0322971000
_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  0.0570
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.388
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94520
_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    1.394
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2627
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         13837
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0602P)^2^+2.8263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8584
_reflns_number_total             13837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03808c2.cif
_cod_data_source_block           Br-010-CCDC-2014810_R1
_cod_depositor_comments
'Adding full bibliography for 7127029--7127048.cif.'
_cod_original_formula_sum        'C48 H70 Br0.60 Cl5.40 Fe2 N2 O15'
_cod_database_code               7127036
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C48 H70 Cl5.40 Br0.60 Fe2 N2 O15'
_reflns_odcompleteness_completeness 91.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.40
_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
 C3-Br1
 1.88 with sigma of 0.02
 C11-Br4
 1.88 with sigma of 0.02
 C8-Br3
 1.88 with sigma of 0.02
 C17-Br6
 1.88 with sigma of 0.02
 C14-Br5
 1.88 with sigma of 0.02
3. Rigid bond restraints
 Cl1, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl5, Cl1, Cl3, Cl6, Cl4
 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 Cl1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Cl5 \\sim Cl1 \\sim Cl3 \\sim Cl6 \\sim Cl4: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(O15) \\sim Ueq: with sigma of 0.08 and sigma for terminal atoms of 0.08
Uanis(O16) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl2) = Uanis(Br2)
5. Others
 Fixed Sof: Cl5(0.902) Cl2(0.9) Cl4(0.898) Cl3(0.898) Cl1(0.9) Cl6(0.902)
 Br4(0.102) Br6(0.098) Br1(0.1) Br5(0.098) Br3(0.102) O15(0.5) O16(0.5) Br2(0.1)
6.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C40(H40A,H40B), C19(H19A,H19B), C31(H31A,H31B), C34(H34A,
 H34B), C22(H22A,H22B), C38(H38A,H38B), C20(H20A,H20B), C23(H23A,H23B),
 C25(H25A,H25B), C28(H28A,H28B), C29(H29A,H29B), C37(H37A,H37B), C26(H26A,H26B),
  C32(H32A,H32B), C41(H41A,H41B)
6.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C21(H21A,H21B,
 H21C), C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C27(H27A,H27B,H27C), C24(H24A,
 H24B,H24C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C45(H45A,H45B,H45C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              33217
_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 1.066
_oxdiff_exptl_absorpt_empirical_full_min 0.909