Construction of spin crossover-fluorescence bifunctional iron(ii) complexes with modified bis(pyrazole)pyridine ligands
Zhao, Guo-Hui; Zhang, Shi-Hui; Yi, Cheng; Liu, Tao; Meng, Yin-Shan; New Journal of Chemistry 47 (2023) 10967–10972; doi:10.1039/D3NJ01431B

data_7062476
_publ_section_title
;
 Construction of spin crossover-fluorescence bifunctional iron(ii)
 complexes with modified bis(pyrazole)pyridine ligands
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10967
_journal_page_last               10972
_journal_paper_doi               10.1039/D3NJ01431B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C58 H38 Fe N10, 2.627(C H2 Cl2), 2(Cl O4)'
_chemical_formula_sum            'C60.62 H43.26 Cl7.26 Fe N10 O8'
_chemical_formula_weight         1352.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-27
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2023-05-01 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                96.619(2)
_cell_angle_beta                 102.0490(10)
_cell_angle_gamma                113.550(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5982(6)
_cell_length_b                   14.4074(7)
_cell_length_c                   17.2229(8)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.63
_cell_volume                     2949.8(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            75707
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.213
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1159 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.8987.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       needle
_exptl_crystal_F_000             1381
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         13508
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0627P)^2^+3.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11389
_reflns_number_total             13508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01431b2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7062474--7062476.cif.'
_cod_database_code               7062476
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl4A-C60A = C60A-Cl3A
 1.7 with sigma of 0.02
 Cl2-C59 = C59-Cl1
 1.7 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl8A \\sim O5A \\sim O6A \\sim O7A \\sim O8A: within 3A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 3A
Cl3A \\sim Cl4A \\sim C60A: within 3A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 3A
Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Cl5A)=Sof(Cl6A)=Sof(C61A)=Sof(H61C)=Sof(H61D)=1-FVAR(1)
 Sof(Cl5)=Sof(Cl6)=Sof(C61)=Sof(H61A)=Sof(H61B)=FVAR(1)
 Sof(Cl3A)=Sof(Cl4A)=Sof(C60A)=Sof(H60C)=Sof(H60D)=1-FVAR(2)
 Sof(Cl3)=Sof(Cl4)=Sof(C60)=Sof(H60A)=Sof(H60B)=FVAR(2)
 Sof(Cl8A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=1-FVAR(3)
 Sof(Cl8)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(3)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=1-FVAR(4)
 Sof(O1)=Sof(O2)=Sof(O3)=FVAR(4)
 Sof(Cl1)=Sof(Cl2)=Sof(C59)=Sof(H59A)=Sof(H59B)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C60(H60A,H60B), C60A(H60C,H60D), C61(H61A,H61B), C61A(H61C,
 H61D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C39(H39), C40(H40), C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
;
_shelx_res_checksum              46683
_olex2_submission_special_instructions 'No special instructions were received'