Site-Selective Photoswitching of Two Distinct Magnetic Chromophores in a Propeller-Like Molecule To Achieve Four Different Magnetic States.
Arczyński, Mirosław; Stanek, Jan; Sieklucka, Barbara; Dunbar, Kim R.; Pinkowicz, Dawid; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b09576

data_4129181
_publ_section_title
;
 Site-Selective Photoswitching of Two Distinct Magnetic Chromophores in a
 Propeller-Like Molecule To Achieve Four Different Magnetic States.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b09576
_journal_year                    2019
_chemical_formula_moiety         'C144 H124 Fe4 N32 W2'
_chemical_formula_sum            'C144 H124 Fe4 N32 W2'
_chemical_formula_weight         2897.87
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-08-02 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.7611(14)
_cell_length_b                   23.7611(14)
_cell_length_c                   63.745(4)
_cell_measurement_reflns_used    9538
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.42
_cell_measurement_theta_min      2.56
_cell_volume                     35990(4)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO Photon 50'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            128647
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.395
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0969 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.7674.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       block
_exptl_crystal_F_000             11712
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.5
_platon_squeeze_details
;
TITL MA1002_Fe4W2_kapII_0m_a.res in I4(1)/a
CELL   23.7611   23.7611   63.7450     90.00     90.00     90.00
SPGR I41/a
Q101 0.391 0.336 0.125 !      19.95 eA-3
Q102 0.796 0.359 0.124 !      13.24 eA-3
Q103 0.412 0.952 0.125 !      12.85 eA-3
C104 0.877 0.268 0.124 !       8.65 eA-3
C105 0.213 0.339 0.077 !       8.17 eA-3
C106 0.572 0.756 0.126 !       7.87 eA-3
C107 0.605 0.961 0.167 !       6.97 eA-3
C108 0.787 0.170 0.168 !       6.44 eA-3
C109 0.477 0.629 0.078 !       5.03 eA-3
Q110 0.397 0.545 0.082 !       4.83 eA-3
Q111 0.906 0.818 0.084 !       4.67 eA-3
Q112 0.703 0.890 0.125 !       4.64 eA-3
C113 0.015 0.177 0.083 !       4.63 eA-3
Q114 0.575 0.350 0.084 !       4.55 eA-3
Q115 0.575 0.853 0.920 !       4.52 eA-3
C116 0.065 0.263 0.082 !       4.34 eA-3
Q117 0.619 0.152 0.673 !       4.15 eA-3
Q118 0.211 0.196 0.125 !       3.96 eA-3
C119 0.485 0.625 0.169 !       3.75 eA-3
Q120 0.804 0.959 0.127 !       3.70 eA-3
C121 0.896 0.267 0.168 !       3.54 eA-3
C122 0.313 0.654 0.173 !       3.53 eA-3
Q123 0.602 0.929 0.126 !       3.46 eA-3
Q124 0.909 0.429 0.129 !       3.15 eA-3
Q125 0.600 0.370 0.167 !       3.13 eA-3
Q126 0.142 0.624 0.125 !       3.02 eA-3
Q127 0.295 0.469 0.083 !       2.92 eA-3
Q128 0.720 0.702 0.167 !       2.86 eA-3
Q129 0.411 0.141 0.130 !       2.84 eA-3
Q130 0.859 0.605 0.076 !       2.80 eA-3
Q131 0.315 0.664 0.082 !       2.80 eA-3
C132 0.419 0.577 0.173 !       2.66 eA-3
C133 0.044 0.150 0.139 !       2.64 eA-3
Q134 0.916 0.126 0.098 !       2.56 eA-3
C135 0.550 0.963 0.177 !       2.56 eA-3
C136 0.515 0.866 0.124 !       2.54 eA-3
C137 0.491 0.656 0.096 !       2.54 eA-3
Q138 0.517 0.961 0.086 !       2.52 eA-3
Q139 0.519 0.484 0.083 !       2.51 eA-3
Q140 0.082 0.039 0.121 !       2.50 eA-3
C141 0.268 0.803 0.059 !       2.46 eA-3
C142 0.522 0.775 0.111 !       2.45 eA-3
Q143 0.300 0.477 0.167 !       2.41 eA-3
Q144 0.804 0.537 0.129 !       2.40 eA-3
Q145 0.502 0.442 0.082 !       2.40 eA-3
Q146 0.755 0.946 0.120 !       2.40 eA-3
Q147 0.115 0.029 0.133 !       2.37 eA-3
C148 0.104 0.297 0.133 !       2.34 eA-3
C149 0.546 0.843 0.106 !       2.34 eA-3
C150 0.424 0.636 0.149 !       2.32 eA-3
Q151 0.907 0.517 0.192 !       2.32 eA-3
C152 0.546 0.648 0.616 !       2.31 eA-3
C153 0.196 0.297 0.073 !       2.29 eA-3
C154 0.718 0.588 0.056 !       2.29 eA-3
C155 1.000 0.249 0.055 !       2.29 eA-3
C156 0.103 0.296 0.145 !       2.28 eA-3
C157 0.578 0.641 0.124 !       2.28 eA-3
Q158 0.076 0.465 0.176 !       2.26 eA-3
Q159 0.452 0.133 0.120 !       2.26 eA-3
C160 0.819 0.159 0.161 !       2.26 eA-3
C161 0.959 0.164 0.131 !       2.25 eA-3
C162 0.271 0.839 0.034 !       2.22 eA-3
C163 0.968 0.304 0.134 !       2.22 eA-3
Q164 0.202 0.273 0.097 !       2.18 eA-3
C165 0.381 0.717 0.152 !       2.17 eA-3
C166 0.881 0.224 0.101 !       2.15 eA-3
C167 0.408 0.713 0.627 !       2.15 eA-3
C168 0.451 0.569 0.152 !       2.15 eA-3
C169 0.820 0.146 0.075 !       2.14 eA-3
C170 0.197 0.261 0.158 !       2.14 eA-3
Q171 0.711 0.980 0.133 !       2.13 eA-3
Q172 0.663 0.767 0.126 !       2.11 eA-3
C173 0.997 0.190 0.186 !       2.10 eA-3
Q174 0.970 0.437 0.192 !       2.09 eA-3
C175 0.077 0.265 0.128 !       2.09 eA-3
C176 0.506 0.736 0.068 !       2.09 eA-3
C177 0.555 0.795 0.098 !       2.06 eA-3
C178 0.421 0.682 0.134 !       2.06 eA-3
Q179 0.360 0.304 0.079 !       2.04 eA-3
Q180 0.140 0.196 0.421 !       2.04 eA-3
Q181 0.559 0.613 0.126 !       2.03 eA-3
Q182 0.391 0.634 0.147 !       2.03 eA-3
Q183 0.955 0.589 0.172 !       2.03 eA-3
C184 0.988 0.106 0.090 !       2.02 eA-3
C185 0.962 0.203 0.130 !       2.02 eA-3
C186 0.484 0.795 0.198 !       2.01 eA-3
C187 0.484 0.511 0.076 !       2.01 eA-3
C188 0.500 0.749 0.058 !       2.00 eA-3
C189 0.430 0.740 0.102 !       2.00 eA-3
C190 0.025 0.247 0.128 !       2.00 eA-3
C191 0.210 0.022 0.233 !       1.99 eA-3
C192 0.422 0.752 0.092 !       1.96 eA-3
Q193 0.395 0.362 0.176 !       1.96 eA-3
Q194 0.658 0.937 0.122 !       1.95 eA-3
C195 0.163 0.323 0.085 !       1.95 eA-3
C196 0.754 0.197 0.072 !       1.95 eA-3
C197 0.251 0.303 0.174 !       1.94 eA-3
C198 0.647 0.673 0.136 !       1.93 eA-3
Q199 0.069 0.142 0.113 !       1.93 eA-3
;
_refine_diff_density_max         4.808
_refine_diff_density_min         -2.537
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         19824
_refine_ls_number_restraints     530
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.1064
_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^)+(0.1806P)^2^+744.3132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2724
_refine_ls_wR_factor_ref         0.3301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14910
_reflns_number_total             19824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09576_si_009.cif
_cod_data_source_block           ma1002_fe4w2_kapii_0m_09__09_proba_sq
_cod_original_cell_volume        35990(5)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4129181
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.495
_shelx_estimated_absorpt_t_min   0.416
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.368(2)
 0.632(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C26-C37
 1.45 with sigma of 0.02
 C70-C59
 1.45 with sigma of 0.02
4. Restrained planarity
 C37, C26, C27, C38, C25, C29, C28, C30, C31, C33, C32, C34, C39, C36, C35,
 C40, N12, N11
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C40 \\sim C35 \\sim C34 \\sim C32 \\sim C39 \\sim C36 \\sim C33 \\sim C31 \\sim
C30 \\sim C28 \\sim C29 \\sim C25 \\sim C26 \\sim C27 \\sim C38 \\sim C37 \\sim
N12 \\sim N11: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C26 \\sim C37: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.014
C40 \\sim C35 \\sim C34 \\sim C39 \\sim C36 \\sim N12 \\sim C33 \\sim C32 \\sim
C31 \\sim C30 \\sim C28 \\sim C29 \\sim N11 \\sim C25 \\sim C26 \\sim C27 \\sim
C38 \\sim C37: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C22 \\sim C11 \\sim C10 \\sim C21 \\sim C9 \\sim C13 \\sim C12 \\sim N9 \\sim
C14 \\sim C15 \\sim C16 \\sim N10 \\sim C17 \\sim C18 \\sim C23 \\sim C20 \\sim
C19 \\sim C24: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C52 \\sim C51 \\sim C50 \\sim C48 \\sim C49 \\sim N14 \\sim C45 \\sim N13 \\sim
C41 \\sim C42 \\sim C53 \\sim C54 \\sim C43 \\sim C44 \\sim C46 \\sim C47 \\sim
C55 \\sim C56: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C60 \\sim C59 \\sim C58 \\sim C57 \\sim N15 \\sim C61 \\sim C65 \\sim N16 \\sim
C68 \\sim C67 \\sim C66 \\sim C64 \\sim C63 \\sim C62 \\sim C70 \\sim C69 \\sim
C71 \\sim C72: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6.a Me refined with riding coordinates:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C69(H69A,H69B,
 H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C40(H40A,H40B,H40C), C39(H39A,
 H39B,H39C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
6.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C46(H46), C47(H47), C62(H62), C63(H63), C68(H68), C25(H25),
 C30(H30), C31(H31), C36(H36), C20(H20), C15(H15), C14(H14), C9(H9)
6.c Fitted hexagon refined as free rotating group:
 C59(C58,C57,N15,C61,C60)
6.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C70(H70A,H70B,H70C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'