Zn-Templated synthesis of substituted (2,6-diimine)pyridine proligands and evaluation of their iron complexes as anolytes for flow battery applications.
Braun, Jason D.; Gray, Paul A.; Sidhu, Baldeep K.; Nemez, Dion B.; Herbert, David E.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16175–16183; doi:10.1039/d0dt00543f

data_7704049
_publ_section_title
;
 Zn-Templated synthesis of substituted (2,6-diimine)pyridine proligands
 and evaluation of their iron complexes as anolytes for flow battery
 applications.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16175
_journal_page_last               16183
_journal_paper_doi               10.1039/d0dt00543f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C21 H17 Br2 Cl2 N3 Zn, 0.5(C2 H3 N)'
_chemical_formula_sum            'C22 H18.5 Br2 Cl2 N3.5 Zn'
_chemical_formula_weight         627.99
_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
_audit_creation_date             2020-01-24
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-10 deposited with the CCDC.	2020-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                92.855(2)
_cell_angle_beta                 110.335(2)
_cell_angle_gamma                102.818(2)
_cell_formula_units_Z            4
_cell_length_a                   12.9613(7)
_cell_length_b                   14.5938(6)
_cell_length_c                   15.1144(7)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.64
_cell_volume                     2588.7(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker D8 Quest ECO CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.1025
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34726
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.721
_diffrn_reflns_theta_min         2.639
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.257
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1137 before and 0.0633 after correction.
The Ratio of minimum to maximum transmission is 0.5097.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.609
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         15756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0093P)^2^+12.0571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9160
_reflns_number_total             15756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00543f2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 7704046--7704050.cif.'
_cod_original_formula_sum        'C22 H18.50 Br2 Cl2 N3.50 Zn'
_cod_database_code               7704049
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.515
_shelx_estimated_absorpt_t_min   0.155
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C14(H14), C15(H15), C17(H17),
 C18(H18), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C32(H32), C33(H33),
  C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              40723
_shelx_fab_checksum              66486
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'