Bidirectional photoswitching of magnetic properties at room temperature: ligand-driven light-induced valence tautomerism
Witt, Alexander; Heinemann, Frank W.; Khusniyarov, Marat M.; Chem. Sci. 6 (2015) 4599–; doi:10.1039/C5SC00130G

data_1519929
_publ_section_title
;
 Bidirectional photoswitching of magnetic properties at room temperature:
 ligand-driven light-induced valence tautomerism
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              4599
_journal_paper_doi               10.1039/C5SC00130G
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C54 H62 Co N2 O4, 4(C7 H8)'
_chemical_formula_sum            'C82 H94 Co N2 O4'
_chemical_formula_weight         1230.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-10 deposited with the CCDC.
2015-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.445(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.5308(6)
_cell_length_b                   11.7257(4)
_cell_length_c                   18.9821(7)
_cell_measurement_reflns_used    9390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.58
_cell_volume                     3510.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            125055
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         1.436
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0474 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.9304.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             1318
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8442
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+2.3151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7474
_reflns_number_total             8442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc00130g2.cif
_cod_data_source_block           aw1501
_cod_depositor_comments
'Adding full bibliography for 1519926--1519929.cif.'
_cod_database_code               1519929
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.866
_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
C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim
C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim C217: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Same fragment restrains
{C101, C102, C103, C104, C105, C106, C107} sigma for 1-2: 0.02, 1-3: 0.04
as
{C201, C202, C203, C204, C205, C206, C207}
{C101, C102, C103, C104, C105, C106, C107} sigma for 1-2: 0.02, 1-3: 0.04
as
{C211, C212, C213, C214, C215, C216, C217}
4. Others
 Sof(C211)=Sof(H211)=Sof(C212)=Sof(H212)=Sof(C213)=Sof(H213)=Sof(C214)=
 Sof(H214)=Sof(C215)=Sof(H215)=Sof(C216)=Sof(C217)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=1-FVAR(1)
 Sof(C201)=Sof(H201)=Sof(C202)=Sof(H202)=Sof(C203)=Sof(H203)=Sof(C204)=
 Sof(H204)=Sof(C205)=Sof(H205)=Sof(C206)=Sof(C207)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C201(H201), C202(H202), C203(H203),
 C204(H204), C205(H205), C211(H211), C212(H212), C213(H213), C214(H214),
 C215(H215)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C107(H10D,H10E,H10F), C207(H20A,H20B,
 H20C), C217(H21A,H21B,H21C)
;
_shelx_res_checksum              8747
_olex2_submission_special_instructions 'No special instructions were received'