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_7704050
_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         'C42 H34 Br4 Fe N6, C2 H3 N, 2(F6 P)'
_chemical_formula_sum            'C44 H37 Br4 F12 Fe N7 P2'
_chemical_formula_weight         1329.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-19
_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                90
_cell_angle_beta                 102.194(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9244(7)
_cell_length_b                   17.5570(7)
_cell_length_c                   15.9880(6)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.66
_cell_volume                     4917.9(3)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            79707
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.617
_diffrn_reflns_theta_min         2.320
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.708
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1017 before and 0.0825 after correction.
The Ratio of minimum to maximum transmission is 0.8120.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.047(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         14968
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0356
_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^)+3.7254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.977
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                12406
_reflns_number_total             14968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00543f2.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7704046--7704050.cif.'
_cod_database_code               7704050
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.510
_shelx_estimated_absorpt_t_min   0.341
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.953(5)
 0.047(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.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)
3.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              1004
_olex2_submission_special_instructions 'No special instructions were received'