A novel bis-1,2,4-benzothiadiazine pincer ligand: synthesis, characterization and first row transition metal complexes.
Pringouri, Konstantina; Anwar, Muhammad U.; Mansour, Liz; Doupnik, Nathan; Beldjoudi, Yassine; Gavey, Emma L.; Pilkington, Melanie; Rawson, Jeremy M.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15725–15736; doi:10.1039/c8dt03346c

data_7047795
_publ_section_title
;
 A novel bis-1,2,4-benzothiadiazine pincer ligand: synthesis,
 characterization and first row transition metal complexes.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15725
_journal_page_last               15736
_journal_paper_doi               10.1039/c8dt03346c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C38 H26 Fe N10 S4, 2(C F3 O3 S), O1, 1.6(C2 H3 N)'
_chemical_formula_sum            'C43.2 H30.8 F6 Fe N11.6 O7 S6'
_chemical_formula_weight         1186.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-20 deposited with the CCDC.
2018-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.5220(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9579(4)
_cell_length_b                   11.0245(4)
_cell_length_c                   22.8045(8)
_cell_measurement_reflns_used    9609
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.96
_cell_volume                     2678.54(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53922
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.947
_diffrn_reflns_theta_max         24.947
_diffrn_reflns_theta_min         2.955
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       lathe
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as 2-component inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9207
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0691P)^2^+3.4328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                8754
_reflns_number_total             9207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03346c2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
'Adding full bibliography for 7047794--7047802.cif.'
_cod_original_formula_sum        'C43.20 H30.80 F6 Fe N11.60 O7 S6'
_cod_database_code               7047795
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.870
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(2)
 0.03(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uiso(N1S) = Uiso(N2S)
Uiso(C2S) = Uiso(C4S)
Uiso(C3S) = Uiso(C5S)
Uiso(O1W) = Uiso(O2W) = Uiso(O3W) = Uiso(O4W) = Uiso(O5W)
4. Others
 1*[Sof(O1W)]+1*[Sof(O2W)]+1*[Sof(O3W)]+1*[Sof(O4W)]+1*[Sof(O5W)]=1 with esd
 of 0
 Fixed Sof: N2S(0.6) C4S(0.6) C5S(0.6) H5SA(0.6) H5SB(0.6) H5SC(0.6)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2A), N5(H5A), N7(H7A), N10(H10A), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9),
 C10(H10), C11(H11), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
  C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35),
 C36(H36), C37(H37)
5.b Idealised Me refined as rotating group:
 C5S(H5SA,H5SB,H5SC), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              2386
_olex2_submission_special_instructions 'No special instructions were received'