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_7062474
_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         'C42 H30 Fe N10, 2(Cl O4)'
_chemical_formula_sum            'C42 H30 Cl2 Fe N10 O8'
_chemical_formula_weight         929.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-01 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1519(13)
_cell_length_b                   11.7439(7)
_cell_length_c                   14.6586(7)
_cell_measurement_reflns_used    8039
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.82
_cell_measurement_theta_min      2.40
_cell_volume                     3813.4(4)
_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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28492
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.869
_diffrn_reflns_theta_min         2.405
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1230 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.8503.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5451
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0375P)^2^+6.7586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3991
_reflns_number_total             5451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01431b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7062474--7062476.cif.'
_cod_database_code               7062474
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
O3: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
1.7A
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) = Uanis(O3A)
3. Others
 Fixed Sof: O3(0.5) O3A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C19(H), C21(Ha), C20(Hb), C12(Hc), C10(Hd), C18(He), C17(Hf), C1(Hg), C6(Hh),
 C15(Hi), C16(Hj), C5(Hk), C9(Hl), C3(Hm), C4(Hn)
;
_shelx_res_checksum              96093
_olex2_submission_special_instructions 'No special instructions were received'