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_7127046
_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
'C18 Cl3.49 F2.51 Fe2 O12, 2(C12 H28 N), 2(C3 H6 O), O'
_chemical_formula_sum            'C48 H70 Cl3.49 F2.51 Fe2 N2 O15'
_chemical_formula_weight         1198.17
_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
_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                 107.210(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6602(8)
_cell_length_b                   22.2123(10)
_cell_length_c                   14.2016(6)
_cell_measurement_reflns_used    19055
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.2680
_cell_measurement_theta_min      2.0940
_cell_volume                     5924.1(5)
_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 0.999
_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      -0.0282173000
_diffrn_orient_matrix_UB_12      0.0153442000
_diffrn_orient_matrix_UB_13      -0.0343966000
_diffrn_orient_matrix_UB_21      0.0250762000
_diffrn_orient_matrix_UB_22      0.0177252000
_diffrn_orient_matrix_UB_23      -0.0147493000
_diffrn_orient_matrix_UB_31      0.0005300000
_diffrn_orient_matrix_UB_32      -0.0216974000
_diffrn_orient_matrix_UB_33      -0.0364890000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41206
_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         25.350
_diffrn_reflns_theta_min         1.818
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91499
_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    1.343
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10838
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1574P)^2^+6.8083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2266
_refine_ls_wR_factor_ref         0.2567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7500
_reflns_number_total             10838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03808c2.cif
_cod_data_source_block           F-042_CCDC-2014822_R1
_cod_depositor_comments
'Adding full bibliography for 7127029--7127048.cif.'
_cod_database_code               7127046
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H70 Cl5.66 F0.34 Fe2 N2 O15'
_reflns_odcompleteness_completeness 90.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.21
_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
 Cl3-C8
 1.73 with sigma of 0.02
 C44-O13
 1.22 with sigma of 0.02
 Cl2-C6
 1.73 with sigma of 0.02
 Cl1-C3
 1.73 with sigma of 0.02
 C6-F2
 1.33 with sigma of 0.02
 C3-F1
 1.33 with sigma of 0.02
 C12-F4
 1.33 with sigma of 0.02
3. Rigid bond restraints
 C45, C44, O13, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O14) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C47) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: Cl6(0.6117) Cl3(0.5317) Cl5(0.6117) Cl2(0.6017) Cl1(0.6017)
 Cl4(0.5317) O15(0.5) O14(0.5) F1(0.3983) F6(0.3883) F4(0.4683) F5(0.3883)
 F2(0.3983) F3(0.4683)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C25(H25A,H25B), C19(H19A,H19B), C28(H28A,H28B), C20(H20A,
 H20B), C29(H29A,H29B), C41(H41A,H41B), C26(H26A,H26B), C23(H23A,H23B),
 C40(H40A,H40B), C34(H34A,H34B), C31(H31A,H31B), C35(H35A,H35B), C37(H37A,H37B),
  C38(H38A,H38B), C32(H32A,H32B)
6.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C24(H24A,H24B,
 H24C), C42(H42A,H42B,H42C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C), C48(H48A,
 H48B,H48C), C47(H47A,H47B,H47C), C39(H39A,H39B,H39C), C43(H43A,H43B,H43C),
 C45(H45A,H45B,H45C)
;
_shelx_res_checksum              96744
_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 1.600
_oxdiff_exptl_absorpt_empirical_full_min 0.631