Substituent effects on the fluorescent spin-crossover Fe(ii) complexes of rhodamine 6G hydrazones
Yuan, Juan; Liu, Mei-Jiao; Wu, Shu-Qi; Zhu, Xin; Zhang, Nan; Sato, Osamu; Kou, Hui-Zhong; Inorganic Chemistry Frontiers 6 (2019) 1170–; doi:10.1039/C9QI00111E

data_4350002
_publ_section_title
;
 Substituent effects on the fluorescent spin-crossover Fe(ii) complexes of
 rhodamine 6G hydrazones
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1170
_journal_paper_doi               10.1039/C9QI00111E
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety
'C64 H62 Fe N10 O4, 2(Cl O4), 2(C H4 O), 1.75(O)'
_chemical_formula_sum            'C66 H73.5 Cl2 Fe N10 O15.75'
_chemical_formula_weight         1385.59
_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             2019-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2019-01-15 deposited with the CCDC.	2019-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.407(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1308(6)
_cell_length_b                   27.8856(14)
_cell_length_c                   22.265(2)
_cell_measurement_reflns_used    5029
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      72.7950
_cell_measurement_theta_min      4.3410
_cell_volume                     6722.5(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -63.00  34.00   1.00    2.64    --  -40.31  38.00  60.00   97
  2  \w     26.00  75.00   1.00    2.64    --   40.31-125.00 -90.00   49
  3  \w     30.00 109.00   1.00   10.50    --  112.00 -95.00 -30.00   79
  4  \w     33.00  72.00   1.00   10.50    --  112.00 -95.00  90.00   39
  5  \w     45.00 109.00   1.00   10.50    --  112.00 -95.00 150.00   64
  6  \w     42.00 133.00   1.00   10.50    --  112.00 -45.00 150.00   91
  7  \w     96.00 123.00   1.00   10.50    --  112.00  30.00 120.00   27
  8  \w    137.00 173.00   1.00   10.50    --  112.00  30.00 120.00   36
  9  \w    133.00 176.00   1.00   10.50    --  112.00  30.00  90.00   43
 10  \w    146.00 172.00   1.00   10.50    --  112.00 111.00 150.00   26
 11  \w    111.00 145.00   1.00   10.50    --  112.00 111.00 150.00   34
 12  \w    108.00 133.00   1.00   10.50    --  112.00 178.00  90.00   25
 13  \w    100.00 152.00   1.00   10.50    --  112.00 111.00 -60.00   52
 14  \w    107.00 160.00   1.00   10.50    --  112.00  45.00  30.00   53
 15  \w     86.00 170.00   1.00   10.50    --  112.00  45.00  60.00   84
 16  \w     57.00  99.00   1.00   10.50    --  112.00 178.00  90.00   42
 17  \w     84.00 133.00   1.00   10.50    --  112.00 -61.00-180.00   49
 18  \w   -112.00   1.00   1.00    2.64    --  -40.31 -19.00-150.00  113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0849694000
_diffrn_orient_matrix_UB_12      -0.0401846000
_diffrn_orient_matrix_UB_13      -0.0332347000
_diffrn_orient_matrix_UB_21      -0.0419326000
_diffrn_orient_matrix_UB_22      -0.0107316000
_diffrn_orient_matrix_UB_23      0.0598703000
_diffrn_orient_matrix_UB_31      -0.1062274000
_diffrn_orient_matrix_UB_32      0.0363634000
_diffrn_orient_matrix_UB_33      -0.0190882000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32734
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         3.770
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic green'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       plate
_exptl_crystal_F_000             2902
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         11415
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1443
_refine_ls_R_factor_gt           0.1048
_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^)+(0.1456P)^2^+11.3503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2835
_refine_ls_wR_factor_ref         0.3135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7144
_reflns_number_total             11415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00111e2.cif
_cod_data_source_block           'global_CCDC2'
_cod_original_cell_volume        6722.6(8)
_cod_original_formula_sum        'C66 H73.50 Cl2 Fe N10 O15.75'
_cod_database_code               4350002
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         FeCNOHCl
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O3W) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C64) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O2W(0.5) O3W(0.25)
4.a Riding coordinates:
 O13(H13), O14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C61(H61A,H61B), C63(H63A,H63B)
4.c Aromatic/amide H refined with riding coordinates:
 N7(H7), N8(H8), N9(H9), N10(H10), C1(H1), C2(H2), C3(H3), C4(H4), C6(H6),
 C9(H9A), C10(H10A), C11(H11), C12(H12), C16(H16), C19(H19), C22(H22), C25(H25),
  C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C41(H41), C42(H42),
 C43(H43), C44(H44), C48(H48), C51(H51), C54(H54), C57(H57)
4.d Idealised Me refined as rotating group:
 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), C66(H66A,H66B,H66C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              78105
_shelx_hkl_checksum              6435
_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 1.914
_oxdiff_exptl_absorpt_empirical_full_min 0.587