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_4129179
_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         2722.06
_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
_audit_creation_date             2018-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4416(4)
_cell_length_b                   23.4416(4)
_cell_length_c                   63.1632(19)
_cell_measurement_reflns_used    13489
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.8200069892
_cell_measurement_theta_min      0.893846581767
_cell_volume                     34708.7(13)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.10.2-g9c23cb36c-release'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.10.2-g9c23cb36c-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.580-g8b4a78df-dials-1.10 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1582
_diffrn_reflns_av_unetI/netI     0.1384
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            151328
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.740
_diffrn_reflns_theta_min         0.898
_diffrn_source                   'Diamond Light Source Beamline I19-2'
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.996564651226
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.058: AIMLESS, version 0.7.1 : 27/03/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       block
_exptl_crystal_F_000             11232
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         22367
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.2232
_refine_ls_R_factor_gt           0.1159
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3530
_refine_ls_wR_factor_ref         0.4033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8239
_reflns_number_total             22367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09576_si_006.cif
_cod_data_source_block           Fe4Mo2_S_170K_FIN
_cod_original_cell_volume        34708.7(16)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4129179
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1
 1.15 with sigma of 0.02
 C2-N2
 1.15 with sigma of 0.02
 C1-N1 = C2-N2
 1.15 with sigma of 0.005
 C1-N1
 1.15 with sigma of 0.008
 C54-C43
 1.55 with sigma of 0.01
 C40-C35
 1.53 with sigma of 0.001
 C34-C40
 2.5 with sigma of 0.001
 C36-C40
 2.5 with sigma of 0.001
 C24-C19
 1.53 with sigma of 0.01
 C23-C18
 1.53 with sigma of 0.02
 C71-C64
 2.53 with sigma of 0.02
 C71-C66
 1.55 with sigma of 0.02
 C71-C67
 2.53 with sigma of 0.02
 C67-C68
 1.39 with sigma of 0.02
 C66-C67
 1.39 with sigma of 0.02
 C38-C27
 1.53 with sigma of 0.01
 C72-C68
 2.53 with sigma of 0.01
 C72-C66
 2.53 with sigma of 0.01
 C72-C67
 1.53 with sigma of 0.02
3. Restrained planarity
 C33, C32, C34, C35, C36, C39, C40
 with sigma of 0.001
 C25, C26, C27, C28, C29, C30, C31, C32, C33, C37, C38, C34, C35, C36, C39,
 C40, N11, N12
 with sigma of 0.001
 C72, C67, C68, C66, C64, C65, C61, C60, C62, C63, C59, C57, C58, C70, C69, C71
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1: within 2A with sigma of 0.006 and sigma for terminal atoms of 0.012
C65 \\sim C64 \\sim C62 \\sim C60 \\sim C61 \\sim C63: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C46 \\sim C45: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C53 \\sim C42 \\sim C43 \\sim C54 \\sim C41: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
C32 \\sim C34 \\sim C35 \\sim C39: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C32 \\sim C34 \\sim C35 \\sim C36 \\sim C40 \\sim C39: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C33 \\sim C32 \\sim C30 \\sim C31 \\sim C28 \\sim C29: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C24 \\sim C19 \\sim C18 \\sim C23: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C26 \\sim C27 \\sim C28 \\sim C25 \\sim C37 \\sim C38: within 2A with sigma of
0.014 and sigma for terminal atoms of 0.02
C68 \\sim C65 \\sim C64 \\sim C66 \\sim C67 \\sim C67 \\sim C72 \\sim C72:
within 2A with sigma of 0.012 and sigma for terminal atoms of 0.018
Uanis(C38) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C70) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C54) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C39) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C24) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C71) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C41(H41), C52(H52), C68(H68), C30(H30), C57(H57), C20(H20), C9(H9),
 C46(H46), C47(H47), C31(H31), C62(H62), C63(H63), C25(H25), C15(H15), C14(H14)
5.b Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C40(H40A,H40B,H40C), C22(H22A,H22B,
 H22C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C69(H69A,H69B,H69C), C39(H39A,
 H39B,H39C), C21(H21A,H21B,H21C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C),
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C71(H71A,H71B,H71C)
;
_shelx_res_checksum              98220
_shelx_hkl_checksum              52652
_shelx_fab_checksum              50111
_olex2_submission_special_instructions 'No special instructions were received'