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_7047801
_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
'2(C19 H13 N5 S2 Zn0.5), 2(C F3 O3 S), C H4 O'
_chemical_formula_sum            'C41 H30 F6 N10 O7 S6 Zn'
_chemical_formula_weight         1146.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.9985(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.6103(9)
_cell_length_b                   11.4305(4)
_cell_length_c                   29.8443(8)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.89
_cell_volume                     9139.1(5)
_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      173.19
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD with Photon detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            110527
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         2.846
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       plate
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.573
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         9368
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0161P)^2^+65.7495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7843
_reflns_number_total             9368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03346c2.cif
_cod_data_source_block           Compound6
_cod_depositor_comments
'Adding full bibliography for 7047794--7047802.cif.'
_cod_database_code               7047801
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.820
_olex2_refinement_description
;
1. 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, All O(H) groups
2. Restrained distances
 S11-O11 = S11-O12 = S11-O13
 1.46241 with sigma of 0.01
 O11-O12 = O11-O13 = O12-O13
 2.388116 with sigma of 0.02
 C0AA-F11 = C0AA-F12 = C0AA-F13
 1.31517 with sigma of 0.01
 F11-F12 = F11-F13 = F12-F13
 2.147673 with sigma of 0.02
 S21-O21A = S21-O21B = S21-O21C
 1.46241 with sigma of 0.01
 O21A-O21B = O21A-O21C = O21B-O21C
 2.388116 with sigma of 0.02
 S22-O22A = S22-O22B = S22-O22C
 1.46241 with sigma of 0.01
 O22A-O22B = O22A-O22C = O22B-O22C
 2.388116 with sigma of 0.02
 C21S-F21A = C21S-F21B = C21S-F21C
 1.31517 with sigma of 0.01
 C22S-F22A = C22S-F22B = C22S-F22C
 1.31517 with sigma of 0.01
 F21A-F21B = F21A-F21C = F21B-F21C
 2.147673 with sigma of 0.02
 F22A-F22B = F22A-F22C = F22B-F22C
 2.147673 with sigma of 0.02
3. Rigid bond restraints
 F22A, F22B, F22C, C22S, C22S, C22S, F21A, F21B, F21C, C21S, C21S, C21S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S22, S22, S22, O22A, O22B, O22C, S21, S21, S21, O21A, O21B, O21C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
S22 \\sim S21: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C22S \\sim C21S: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O21A) = Uanis(O21B) = Uanis(O21C) = Uanis(O22A) = Uanis(O22B) =
Uanis(O22C)
5. Others
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(2)
 1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(3)
 Fixed Sof: S22(0.5) F22A(0.5) F22B(0.5) F22C(0.5) O22A(0.5) O22B(0.5)
 O22C(0.5) C22S(0.5) S21(0.5) F21A(0.5) F21B(0.5) F21C(0.5) O21A(0.5) O21B(0.5)
 O21C(0.5) C21S(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2A), N5(H5A), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11),
 C15(H15), C16(H16), C17(H17), C18(H18), N7(H7A), N10(H10A), C21(H21), C22(H22),
  C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35),
 C36(H36), C37(H37)
6.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
6.c Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              16062
_olex2_submission_special_instructions 'No special instructions were received'