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_4129184
_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 H128 Fe4 Mo2 N32'
_chemical_formula_sum            'C144 H128 Fe4 Mo2 N32'
_chemical_formula_weight         2722.07
_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             2017-07-26
_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                   23.7526(5)
_cell_length_b                   23.7526(5)
_cell_length_c                   63.7037(16)
_cell_measurement_reflns_used    28842
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.78
_cell_volume                     35940.7(14)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0722
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            97219
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.039
_diffrn_reflns_theta_max         25.039
_diffrn_reflns_theta_min         2.508
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0765 before and 0.0597 after correction. The Ratio of minimum to maximum transmission is 0.8690. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_description       block
_exptl_crystal_F_000             11232
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.39
_platon_squeeze_details
;
TITL MA995_Fe4Mo2_kapII_0m_a.res in I4(1)/a
CELL   23.7526   23.7526   63.7037     90.00     90.00     90.00
SPGR I41/a
C101 0.055 0.031 0.081 !       2.94 eA-3
C102 0.064 0.988 0.067 !       2.74 eA-3
C103 0.272 0.346 0.051 !       1.94 eA-3
C104 0.437 0.502 0.191 !       1.77 eA-3
C105 0.459 0.491 0.066 !       1.69 eA-3
C106 0.717 0.734 0.170 !       1.59 eA-3
C107 0.542 0.905 0.101 !       1.53 eA-3
C108 0.432 0.525 0.184 !       1.51 eA-3
C109 0.705 0.683 0.168 !       1.38 eA-3
C110 0.784 0.141 0.079 !       1.37 eA-3
C111 0.250 0.801 0.009 !       1.34 eA-3
C112 1.002 0.132 0.087 !       1.22 eA-3
C113 0.578 0.962 0.171 !       1.16 eA-3
C114 0.272 0.335-0.001 !       1.10 eA-3
C115 0.258 0.834 0.017 !       1.02 eA-3
C116 0.382 0.485 0.205 !       1.02 eA-3
C117 0.714 0.008 0.229 !       1.01 eA-3
Q118 0.649 0.035 0.202 !       1.00 eA-3
C119 0.266 0.514 0.230 !       0.96 eA-3
C120 0.941 0.272 0.056 !       0.95 eA-3
C121 0.104 0.269 0.144 !       0.95 eA-3
C122 0.234 0.461 0.021 !       0.95 eA-3
C123 0.966 0.403 0.109 !       0.95 eA-3
C124 0.255 0.105 0.000 !       0.94 eA-3
C125 0.719 0.634 0.015 !       0.94 eA-3
C126 0.764 0.491 0.238 !       0.92 eA-3
C127 0.258 0.062 0.001 !       0.92 eA-3
C128 0.196 1.000 0.214 !       0.91 eA-3
C129 0.259 0.969 0.034 !       0.90 eA-3
C130 0.632 0.702 0.130 !       0.89 eA-3
C131 0.500 0.868 0.078 !       0.88 eA-3
C132 0.458 0.637 0.116 !       0.88 eA-3
C133 0.349 0.027 0.238 !       0.88 eA-3
C134 0.696 0.970 0.227 !       0.86 eA-3
C135 0.229 0.550 0.012 !       0.84 eA-3
C136 0.214 0.442 0.030 !       0.84 eA-3
C137 0.828 0.984 0.238 !       0.84 eA-3
C138 0.981 0.231 0.199 !       0.84 eA-3
C139 0.500 0.752 0.199 !       0.83 eA-3
C140 0.765 0.466 0.001 !       0.83 eA-3
C141 0.774 0.519 0.028 !       0.83 eA-3
C142 0.234 0.038 0.224 !       0.83 eA-3
C143 0.694 0.022 0.201 !       0.81 eA-3
C144 0.610 0.729 0.157 !       0.81 eA-3
C145 0.150 0.020 0.219 !       0.81 eA-3
C146 0.744 0.475 0.236 !       0.79 eA-3
C147 0.705 0.478 0.222 !       0.79 eA-3
C148 0.328 0.990 0.238 !       0.78 eA-3
C149 0.430 0.726 0.058 !       0.78 eA-3
C150 0.889 0.482 0.242 !       0.78 eA-3
C151 0.740 0.089 0.041 !       0.77 eA-3
C152 0.956 0.214 0.199 !       0.77 eA-3
C153 0.243 1.000 0.031 !       0.77 eA-3
C154 0.257 0.500 0.469 !       0.77 eA-3
C155 0.267 0.762 0.017 !       0.76 eA-3
C156 0.232 0.422 0.024 !       0.76 eA-3
C157 0.250 0.005 0.785 !       0.76 eA-3
C158 0.717 0.514 0.238 !       0.76 eA-3
C159 0.190 0.478 0.238 !       0.76 eA-3
C160 0.679 0.999 0.764 !       0.75 eA-3
C161 0.783 0.472 0.211 !       0.75 eA-3
C162 0.846 0.272 0.160 !       0.75 eA-3
C163 0.203 0.970 0.234 !       0.74 eA-3
C164 0.022 0.238 0.191 !       0.74 eA-3
C165 0.752 0.876 0.009 !       0.73 eA-3
C166 0.613 0.701 0.176 !       0.73 eA-3
C167 0.613 0.205 0.824 !       0.73 eA-3
C168 0.530 0.716 0.195 !       0.72 eA-3
C169 0.795 0.965 0.025 !       0.71 eA-3
C170 0.272 0.957 0.247 !       0.70 eA-3
C171 0.257 0.925 0.035 !       0.69 eA-3
C172 0.788 0.558 0.015 !       0.69 eA-3
C173 0.423 0.813 0.180 !       0.68 eA-3
C174 0.806 0.161 0.052 !       0.68 eA-3
C175 0.263 0.976 0.005 !       0.68 eA-3
C176 0.013 0.082 0.098 !       0.68 eA-3
C177 0.607 0.804 0.074 !       0.67 eA-3
C178 0.534 0.358 0.933 !       0.66 eA-3
C179 0.676 0.553 0.019 !       0.65 eA-3
C180 0.687 0.973 0.211 !       0.65 eA-3
C181 0.203 0.990 0.245 !       0.65 eA-3
C182 0.229 0.519 0.226 !       0.65 eA-3
C183 0.140 0.984 0.234 !       0.64 eA-3
C184 0.454 0.854 0.075 !       0.63 eA-3
C185 0.782 0.444 0.243 !       0.63 eA-3
C186 0.721 0.470 0.009 !       0.63 eA-3
Q187 0.595 0.149 0.125 !       0.63 eA-3
C188 0.500 0.786 0.200 !       0.63 eA-3
Q189 0.701 0.927 0.247 !       0.62 eA-3
C190 0.788 0.131 0.020 !       0.62 eA-3
C191 0.883 0.477 0.219 !       0.62 eA-3
C192 0.404 0.804 0.158 !       0.61 eA-3
C193 0.897 0.504 0.227 !       0.61 eA-3
Q194 0.593 0.498 0.233 !       0.61 eA-3
C195 0.620 0.828 0.078 !       0.60 eA-3
C196 0.718 0.946 0.215 !       0.60 eA-3
C197 0.940 0.346 0.097 !       0.60 eA-3
C198 0.938 0.221 0.067 !       0.59 eA-3
C199 0.787 0.007 0.000 !       0.59 eA-3
;
_refine_diff_density_max         0.718
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         15866
_refine_ls_number_restraints     326
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1221P)^2^+88.0305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.2465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9118
_reflns_number_total             15866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09576_si_002.cif
_cod_data_source_block           ma995_fe4mo2_kapii_0m_a_06__sq
_cod_original_cell_volume        35940.7(18)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4129184
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.807
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9908(7)
 0.0092(7)
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
 C23-C18
 1.45 with sigma of 0.06
 C34-C39
 1.45 with sigma of 0.06
 C40-C35
 1.45 with sigma of 0.02
 C26-C37
 1.45 with sigma of 0.01
 C27-C38
 1.45 with sigma of 0.001
 C24-C19
 1.45 with sigma of 0.06
4. Restrained planarity
 C37, C26, C27, C38, C25, C29, C28, C30, C31, C32, C33, C34, C35, C36, C40,
 C39, N11, N12
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C69 \\sim N15 \\sim C61 \\sim C65 \\sim C57 \\sim C67 \\sim C64 \\sim C66 \\sim
C68 \\sim C71 \\sim C63 \\sim C62 \\sim C58 \\sim C60 \\sim C70 \\sim C72 \\sim
C59: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C49 \\sim C52 \\sim C48 \\sim C55 \\sim C56 \\sim C50 \\sim C51: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C69 \\sim C61 \\sim C65 \\sim C57 \\sim C67 \\sim C64 \\sim C66 \\sim C68 \\sim
C71 \\sim C63 \\sim C62 \\sim C58 \\sim C60 \\sim C70 \\sim C72 \\sim C59:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C69 \\sim C58 \\sim C70 \\sim C59 \\sim C57 \\sim C60: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C39 \\sim C34: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C39 \\sim C34 \\sim C35 \\sim C40: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C25 \\sim C26: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C38 \\sim C37 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C38 \\sim C37 \\sim C36 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim
C32 \\sim C34 \\sim C35 \\sim C39 \\sim C33 \\sim C40 \\sim C31 \\sim C30:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C38 \\sim C27 \\sim C37 \\sim C26: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C20 \\sim C17 \\sim C18 \\sim C19 \\sim C24 \\sim C16 \\sim C23: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C19 \\sim C24: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq: with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
6.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C41(H41), C47(H47), C36(H36), C46(H46), C25(H25), C57(H57), C9(H9),
 C52(H52), C68(H68), C63(H63), C62(H62), C14(H14), C15(H15), C31(H31), C30(H30)
6.b Fitted hexagon refined as free rotating group:
 C25(C26,C27,C28,C29,N11)
6.c Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C53(H53A,H53B,
 H53C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C), C71(H71A,H71B,H71C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C),
 C70(H70A,H70B,H70C), C39(H39A,H39B,H39C), C72(H72A,H72B,H72C), C40(H40A,H40B,
 H40C), C54(H54A,H54B,H54C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'