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_4350000
_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 H60 Br2 Fe N10 O4, 2(Cl O4), C H2 Cl2, 3(C H4 O), O'
_chemical_formula_sum            'C68 H76 Br2 Cl4 Fe N10 O16'
_chemical_formula_weight         1646.85
_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   geom
_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                 94.094(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2940(6)
_cell_length_b                   28.6311(9)
_cell_length_c                   12.6951(3)
_cell_measurement_reflns_used    13166
_cell_measurement_temperature    110.0(6)
_cell_measurement_theta_max      76.1010
_cell_measurement_theta_min      3.7620
_cell_volume                     7357.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      110.0(6)
_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   -121.00   0.00   1.00    2.50    --  -40.56 -19.00-120.00  121
  2  \w     21.00  81.00   1.00    2.50    --   40.56 -99.00 -90.00   60
  3  \w      9.00  71.00   1.00    2.50    --   40.56 -99.00-180.00   62
  4  \w     94.00 174.00   1.00    6.00    --  111.58 125.00 120.00   80
  5  \w     83.00 127.00   1.00    6.00    --  111.58  30.00 120.00   44
  6  \w    147.00 174.00   1.00    6.00    --  111.58  30.00 120.00   27
  7  \w     40.00 108.00   1.00    6.00    --  111.58 -95.00  60.00   68
  8  \w     60.00 141.00   1.00    6.00    --  111.58 -61.00 120.00   81
  9  \w     51.00  77.00   1.00    6.00    --  111.58-126.00  18.00   26
 10  \w     93.00 118.00   1.00    6.00    --  111.58-126.00  18.00   25
 11  \w     45.00  91.00   1.00    6.00    --  111.58-125.00-180.00   46
 12  \w     95.00 155.00   1.00    6.00    --  111.58  45.00  30.00   60
 13  \w    144.00 178.00   1.00    6.00    --  111.58  45.00 -90.00   34
;
_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      -0.0632805000
_diffrn_orient_matrix_UB_12      -0.0292144000
_diffrn_orient_matrix_UB_13      -0.0212853000
_diffrn_orient_matrix_UB_21      0.0400069000
_diffrn_orient_matrix_UB_22      -0.0450448000
_diffrn_orient_matrix_UB_23      0.0229335000
_diffrn_orient_matrix_UB_31      -0.0136558000
_diffrn_orient_matrix_UB_32      0.0035397000
_diffrn_orient_matrix_UB_33      0.1175804000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27790
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        64.997
_diffrn_reflns_theta_max         64.997
_diffrn_reflns_theta_min         3.782
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.856
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.939
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         12487
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0925
_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^)+(0.1594P)^2^+17.3347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2547
_refine_ls_wR_factor_ref         0.2662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10550
_reflns_number_total             12487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00111e2.cif
_cod_data_source_block           global
_cod_database_code               4350000
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Br Cl Fe'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N10-C63 = C63-C64
 1.48 with sigma of 0.02
 N10-C64
 2.5 with sigma of 0.02
3. Rigid bond restraints
 C63, C64
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C53, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C63 \\sim C64 \\sim N10: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(N10) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O10A) \\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(O12A) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(C60) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(O1WA)=1-FVAR(1)
 Sof(O1W)=FVAR(1)
 Sof(O10A)=Sof(O11A)=Sof(O12A)=1-FVAR(2)
 Sof(O10)=Sof(O11)=Sof(O12)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C61(H61A,H61B), C63(H63A,H63B), C67(H67A,H67B)
6.b Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C)
6.c Aromatic/amide H refined with riding coordinates:
 N7(H7), N8(H8), N9(H9), N10(H10), C2(H2), C3(H3), C4(H4), C6(H6), C10(H10A),
 C11(H11), C12(H12), C9(H9A), 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)
6.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C)
6.e Idealised tetrahedral OH refined as rotating group:
 O13(H13), O14(H14), O15(H15)
;
_shelx_res_checksum              20707
_shelx_hkl_checksum              41024
_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 3.880
_oxdiff_exptl_absorpt_empirical_full_min 0.461