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_7047798
_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         'C19 H13 N5 S2'
_chemical_formula_sum            'C19 H13 N5 S2'
_chemical_formula_weight         375.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-01 deposited with the CCDC.
2018-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                102.372(19)
_cell_angle_beta                 94.93(2)
_cell_angle_gamma                107.958(17)
_cell_formula_units_Z            4
_cell_length_a                   11.185(4)
_cell_length_b                   12.015(5)
_cell_length_c                   13.609(8)
_cell_measurement_reflns_used    9529
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.445
_cell_measurement_theta_min      3.083
_cell_volume                     1676.5(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            62120
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         3.088
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0636 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.9337. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0254P)^2^+3.5298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5555
_reflns_number_total             6843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03346c2.cif
_cod_data_source_block           LH2
_cod_depositor_comments
'Adding full bibliography for 7047794--7047802.cif.'
_cod_original_cell_volume        1676.4(14)
_cod_database_code               7047798
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C2(H2A), C3(H3), C4(H4), C5(H5A), C9(H9), C10(H10), C11(H11),
 C15(H15), C16(H16), C17(H17), C18(H18), N7(H7), N10(H10A), C21(H21), C22(H22),
 C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
  C37(H37)
;
_shelx_res_checksum              53404
_olex2_submission_special_instructions 'No special instructions were received'