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_7127033
_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
'Br2.12 C18 Cl3.88 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Br2.12 Cl3.88 Fe2 N2 O15'
_chemical_formula_weight         1333.71
_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     dual
_audit_creation_date             2020-08-01
_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                 107.935(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3278(4)
_cell_length_b                   21.7798(3)
_cell_length_c                   14.4219(3)
_cell_measurement_reflns_used    24741
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      31.3920
_cell_measurement_theta_min      1.7410
_cell_volume                     6074.8(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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      -0.0313101000
_diffrn_orient_matrix_UB_12      0.0162833000
_diffrn_orient_matrix_UB_13      -0.0207428000
_diffrn_orient_matrix_UB_21      -0.0190729000
_diffrn_orient_matrix_UB_22      -0.0269691000
_diffrn_orient_matrix_UB_23      0.0019508000
_diffrn_orient_matrix_UB_31      -0.0005982000
_diffrn_orient_matrix_UB_32      0.0082328000
_diffrn_orient_matrix_UB_33      0.0473322000
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41976
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.754
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90060
_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    1.458
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2737
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         11085
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0553P)^2^+5.4512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8830
_reflns_number_total             11085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03808c2.cif
_cod_data_source_block           Br-035_CCDC-2014806_R1
_cod_depositor_comments
'Adding full bibliography for 7127029--7127048.cif.'
_cod_database_code               7127033
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C48 H70 Cl3.88 Br2.12 Fe2 N2 O15'
_reflns_odcompleteness_completeness 90.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.37
_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
 Cl1-C3
 1.73 with sigma of 0.02
 C17-Cl6
 1.73 with sigma of 0.02
 Cl3-C8
 1.73 with sigma of 0.02
 Cl2-C6
 1.73 with sigma of 0.02
 C11-Br4
 1.88 with sigma of 0.02
 Cl5-C14
 1.73 with sigma of 0.02
 C17-Br6
 1.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O16) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O15) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(Cl1) = Uanis(Br1)
4. Others
 Fixed Sof: Cl6(0.642) Cl1(0.656) Cl3(0.642) Cl4(0.642) Cl5(0.642) Cl2(0.656)
 O16(0.5) O15(0.5) Br2(0.344) Br5(0.358) Br6(0.358) Br3(0.358) Br1(0.344)
 Br4(0.358)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C22(H22A,H22B), C34(H34A,H34B), C41(H41A,H41B), C40(H40A,
 H40B), C20(H20A,H20B), C29(H29A,H29B), C19(H19A,H19B), C31(H31A,H31B),
 C28(H28A,H28B), C35(H35A,H35B), C26(H26A,H26B), C37(H37A,H37B), C23(H23A,H23B),
  C32(H32A,H32B), C38(H38A,H38B)
5.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C30(H30A,H30B,
 H30C), C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C33(H33A,H33B,H33C), C44(H44A,H44B,H44C),
 C47(H47A,H47B,H47C)
;
_shelx_res_checksum              71009
_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 1.103
_oxdiff_exptl_absorpt_empirical_full_min 0.914