Binuclear coordination complex of open merocyanine form of photochromic spiropyran with MnII(hfac)2 having high spin (S = 5) ground state
Osipov, Nikita G.; Faraonov, Maxim A.; Shestakov, Alexander F.; Mikhailenko, Maxim V.; Kuzmin, Alexey V.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Konarev, Dmitri V.; New Journal of Chemistry 47 (2023) 5470–5476; doi:10.1039/D3NJ00058C

data_7062275
_publ_section_title
;
 Binuclear coordination complex of open merocyanine form of photochromic
 spiropyran with MnII(hfac)2 having high spin (S = 5) ground state
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5470
_journal_page_last               5476
_journal_paper_doi               10.1039/D3NJ00058C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C66 H46 F24 Mn2 N2 O10'
_chemical_formula_sum            'C66 H46 F24 Mn2 N2 O10'
_chemical_formula_weight         1592.93
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-06
_audit_creation_method
;FinalCif V114 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.005(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9995(5)
_cell_length_b                   24.4727(16)
_cell_length_c                   12.1970(5)
_cell_measurement_reflns_used    4158
_cell_measurement_temperature    102(3)
_cell_measurement_theta_max      28.0510
_cell_measurement_theta_min      2.4640
_cell_volume                     3282.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -17.00  21.00   1.00  150.00    --  -12.05 -77.00 120.00   38
  2  \w    -44.00  17.00   1.00  150.00    --  -12.05  77.00   0.00   61
  3  \w     17.00  46.00   1.00  150.00    --   12.05 -77.00 120.00   29
  4  \w    -28.00  60.00   1.00  150.00    --   12.05  19.00 -60.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0426082000
_diffrn_orient_matrix_UB_12      -0.0111235000
_diffrn_orient_matrix_UB_13      -0.0381693000
_diffrn_orient_matrix_UB_21      0.0167767000
_diffrn_orient_matrix_UB_22      -0.0267715000
_diffrn_orient_matrix_UB_23      0.0166677000
_diffrn_orient_matrix_UB_31      -0.0454262000
_diffrn_orient_matrix_UB_32      0.0005539000
_diffrn_orient_matrix_UB_33      0.0405530000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.1008
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17540
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.664
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       plate
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+5.7507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4593
_reflns_number_total             6801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00058c2.cif
_cod_data_source_block           exp_2480_int1
_cod_depositor_comments          'Adding full bibliography for 7062275.cif.'
_cod_database_code               7062275
_chemical_oxdiff_formula         'C132  H92  N4  O20  F48  Mn4  '
_shelx_shelxl_version_number     2018/3
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C16(H16),
 C17(H17), C18(H18), C19(H19), C26(H26), C31(H31)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.123
_oxdiff_exptl_absorpt_empirical_full_min 0.884
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              9017