Rhodamine 6G-Labeled Pyridyl Aroylhydrazone Fe(II) Complex Exhibiting Synergetic Spin Crossover and Fluorescence.
Yuan, Juan; Wu, Shu-Qi; Liu, Mei-Jiao; Sato, Osamu; Kou, Hui-Zhong; Journal of the American Chemical Society 140 (2018) 9426–9433; doi:10.1021/jacs.8b00103

data_4132009
_publ_section_title
;
 Rhodamine 6G-Labeled Pyridyl Aroylhydrazone Fe(II) Complex Exhibiting
 Synergetic Spin Crossover and Fluorescence.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9426
_journal_page_last               9433
_journal_paper_doi               10.1021/jacs.8b00103
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'C66 H66 Fe N10 O4, C H2 Cl2, 2(Cl O4), 0.8(O), 3(C H4 O)'
_chemical_formula_sum            'C70 H81.6 Cl4 Fe N10 O15.8'
_chemical_formula_weight         1513.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.822(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5660(5)
_cell_length_b                   28.5805(8)
_cell_length_c                   12.7724(3)
_cell_measurement_reflns_used    8068
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      74.4610
_cell_measurement_theta_min      4.1980
_cell_volume                     7480.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_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    -61.00 -23.00   1.00    6.00    --  -40.81  57.00 -30.00   38
  2  \w    -91.00  36.00   1.00    6.00    --  -40.81   0.00-180.00  127
  3  \w     31.00  96.00   1.00    6.00    --   40.81-125.00 120.00   65
  4  \w     44.00 121.00   1.00   24.50    --  107.37-125.00   0.00   77
  5  \w     49.00 108.00   1.00   24.50    --  107.37-125.00-120.00   59
  6  \w     89.00 173.00   1.00   24.50    --  107.37  30.00  90.00   84
  7  \w     88.00 157.00   1.00   24.50    --  107.37  30.00-150.00   69
  8  \w    105.00 171.00   1.00   24.50    --  107.37 125.00-120.00   66
  9  \w     51.00 119.00   1.00   24.50    --  107.37 -61.00 -60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0275772000
_diffrn_orient_matrix_UB_12      -0.0427880000
_diffrn_orient_matrix_UB_13      -0.0622900000
_diffrn_orient_matrix_UB_21      0.0550084000
_diffrn_orient_matrix_UB_22      -0.0306405000
_diffrn_orient_matrix_UB_23      0.0528772000
_diffrn_orient_matrix_UB_31      -0.0431772000
_diffrn_orient_matrix_UB_32      -0.0117001000
_diffrn_orient_matrix_UB_33      0.0893186000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29246
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.214
_diffrn_reflns_theta_min         3.771
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       cube
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         14867
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1792P)^2^+2.9438P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2455
_refine_ls_wR_factor_ref         0.2727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10759
_reflns_number_total             14867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00103_si_002.cif
_cod_data_source_block           1-250k
_cod_original_formula_sum        'C70 H81.60 Cl4 Fe N10 O15.80'
_cod_database_code               4132009
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H N O Fe Cl'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Cl2, Cl2A}
3. Restrained distances
 Cl1A-O5A = Cl1A-O6A = Cl1A-O7A = Cl1A-O8A
 1.44 with sigma of 0.01
 O5A-O6A = O5A-O7A = O5A-O8A = O6A-O7A = O6A-O8A = O7A-O8A
 2.35 with sigma of 0.02
4. Rigid bond restraints
 O4, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(O8A)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(O1W) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(Cl1A) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(O11A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O5A)
\\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(O10A) \\sim Ueq, Uanis(O6)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl2) = Uanis(Cl2A)
6. Others
 Sof(Cl2A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=1-FVAR(1)
 Sof(Cl2)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(O9)=FVAR(1)
 Fixed Sof: Cl1(0.8) O5(0.8) O6(0.8) O7(0.8) O8(0.8) O1W(0.8) Cl1A(0.2)
 O5A(0.2) O6A(0.2) O7A(0.2) O8A(0.2)
7.a Riding coordinates:
 O13(H13A), O14(H14), O15(H15)
7.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C61(H61A,H61B), C63(H63A,H63B), C67(H67A,H67B)
7.c Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C)
7.d Aromatic/amide H refined with riding coordinates:
 N7(H7), N8(H8), N9(H9), N10(H10), C2(H2), C3(H3), C4(H4), C6(H6), C9(H9A),
 C10(H10A), C11(H11), C13(H13), C16(H16), C19(H19), C22(H22), C25(H25),
 C34(H34), C35(H35), C36(H36), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44),
  C48(H48), C51(H51), C54(H54), C57(H57)
7.e Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C)
;
_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 2.929
_oxdiff_exptl_absorpt_empirical_full_min 0.508