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_4129183
_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             2018-08-20
_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                   23.1624(3)
_cell_length_b                   23.1624(3)
_cell_length_c                   62.6742(12)
_cell_measurement_reflns_used    19737
_cell_measurement_temperature    30
_cell_measurement_theta_max      28.5014748538
_cell_measurement_theta_min      0.921013522584
_cell_volume                     33624.5(9)
_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      30
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_av_unetI/netI     0.1001
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            148431
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         28.680
_diffrn_reflns_theta_min         1.260
_exptl_absorpt_coefficient_mu    0.484
_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    1.075
_exptl_crystal_description       block
_exptl_crystal_F_000             11232
_refine_diff_density_max         2.305
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         22793
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.1629
_refine_ls_R_factor_gt           0.0938
_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^)+(0.1654P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2746
_refine_ls_wR_factor_ref         0.3118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11660
_reflns_number_total             22793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09576_si_003.cif
_cod_data_source_block           Fe4Mo2_S_30K_sq
_cod_original_cell_volume        33624.5(11)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4129183
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   1.0
_shelx_estimated_absorpt_t_min   0.993266000587
_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. Uiso/Uaniso restraints and constraints
C52 \\sim C51 \\sim C50 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C61 \\sim
N15 \\sim C57 \\sim C58 \\sim C59 \\sim C59 \\sim C60 \\sim C55 \\sim C65 \\sim
C30 \\sim C64 \\sim C56 \\sim C63 \\sim C37 \\sim C31 \\sim C38 \\sim C62 \\sim
C70 \\sim C70 \\sim C69 \\sim C14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.015
N14 \\sim C52 \\sim C51 \\sim C50 \\sim C48 \\sim C49: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C71) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N14) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C50)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C52(H52), C14(H14), C15(H15), C20(H20), C25(H25), C30(H30), C31(H31),
 C36(H36), C41(H41), C46(H46), C47(H47), C57(H57), C62(H62), C63(H63), C68(H68)
3.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39C,H39A,H39B), C40(H40A,
 H40B,H40C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C56(H56A,H56B,H56C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C)
;
_shelx_res_checksum              3093
_shelx_hkl_checksum              71259
_shelx_fab_checksum              30989
_olex2_submission_special_instructions 'No special instructions were received'