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_4350001
_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             2019-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2019-01-24 deposited with the CCDC.	2019-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.166(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3424(6)
_cell_length_b                   28.6600(9)
_cell_length_c                   12.6888(3)
_cell_measurement_reflns_used    7867
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.8510
_cell_measurement_theta_min      3.4925
_cell_volume                     7378.2(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28031
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        64.999
_diffrn_reflns_theta_max         64.999
_diffrn_reflns_theta_min         3.776
_exptl_absorpt_coefficient_mu    4.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60276
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       cube
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.401
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         12539
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1681P)^2^+18.9534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2602
_refine_ls_wR_factor_ref         0.2802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9823
_reflns_number_total             12539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00111e2.cif
_cod_data_source_block           'global_CCDC1'
_cod_database_code               4350001
_shelx_shelxl_version_number     2014/7
_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-C64
 2.48 with sigma of 0.02
 C63-C64
 1.5 with sigma of 0.01
 N10-C63
 1.46 with sigma of 0.01
3. Rigid bond restraints
 C53, O4, Cl2, O12A, C63, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N10) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(Cl2) \\sim Ueq, Uanis(O1WA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O10A) \\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(O12A) \\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 0.001
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)
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), C64(H64A,H64B,H64C), 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              63335
_shelx_hkl_checksum              64839
_olex2_submission_special_instructions 'No special instructions were received'