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_4129180
_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                   23.17950(6)
_cell_length_b                   23.17950(6)
_cell_length_c                   62.6916(3)
_cell_measurement_reflns_used    6545
_cell_measurement_temperature    30(2)
_cell_measurement_theta_max      20.6557631617
_cell_measurement_theta_min      1.24778816742
_cell_volume                     33683.5(2)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      30(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1404
_diffrn_reflns_av_unetI/netI     0.1257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            145412
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.340
_diffrn_reflns_theta_min         1.259
_diffrn_source                   'Diamond Light Source Beamline I19-2'
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.996424305546
_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_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_description       block
_exptl_crystal_F_000             11232
_refine_diff_density_max         1.098
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         20902
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.2472
_refine_ls_R_factor_gt           0.1344
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3965
_refine_ls_wR_factor_ref         0.4420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7257
_reflns_number_total             20902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09576_si_004.cif
_cod_data_source_block           Fe4Mo2_S_30K_405nm_sq_FIN
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4129180
_shelx_shelxl_version_number     2016/6
_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
 C29-C33
 1.35 with sigma of 0.02
 C30-C28
 1.35 with sigma of 0.02
 C32-C31
 1.35 with sigma of 0.02
 C31-C30
 1.35 with sigma of 0.02
 C65-C64
 1.35 with sigma of 0.02
 C32-C33
 1.35 with sigma of 0.02
 C29-C28
 1.35 with sigma of 0.02
 C28-C30
 1.35 with sigma of 0.02
 C62-C63
 1.35 with sigma of 0.02
 C63-C64
 1.35 with sigma of 0.02
 C60-C62
 1.35 with sigma of 0.02
 C27-C38
 1.53 with sigma of 0.02
 C26-C37
 1.53 with sigma of 0.02
 C58-C69
 1.53 with sigma of 0.02
 C10-C21
 1.53 with sigma of 0.02
 C59-C70
 1.53 with sigma of 0.02
 C21-C10
 1.53 with sigma of 0.02
 C50-C55
 1.53 with sigma of 0.02
3. Restrained planarity
 C68, C61, C57, C58, C59, C60, C67, C65, C66, C72, C64, C63, C62, C71, C69, C70
 with sigma of 0.01
 N12, N12, C36, C35, C33, C33, C32, C30, C34, C31, C37, C39, C40, C38, C29,
 C25, C26, C27, C28
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C68 \\sim C61 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C67 \\sim C65 \\sim
C66 \\sim C72 \\sim C64 \\sim C63 \\sim C62 \\sim C71 \\sim C69 \\sim C70:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C36 \\sim C35 \\sim C33 \\sim C32 \\sim C30 \\sim C34 \\sim C31 \\sim C37 \\sim
C39 \\sim C40 \\sim C38 \\sim C29 \\sim C26 \\sim C27 \\sim C28: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.03
Uanis(C70) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C52) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C52(H52), C47(H47), C46(H46), C41(H41), C68(H68), C63(H63), C62(H62),
 C57(H57), C20(H20), C15(H15), C14(H14), C9(H9), C36(H36), C31(H31), C30(H30),
 C25(H25)
5.b Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C53(H53A,H53B,
 H53C), C72(H72A,H72B,H72C), C71(H71A,H71B,H71C), C70(H70A,H70B,H70C), C69(H69A,
 H69B,H69C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C),
 C21(H21A,H21B,H21C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C38(H38A,H38B,
 H38C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              2718
_shelx_hkl_checksum              99843
_shelx_fab_checksum              64122
_olex2_submission_special_instructions 'No special instructions were received'