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_7047797
_publ_section_title
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 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 N10 Ni S4, 2(Cl), 4(C H4 O)'
_chemical_formula_sum            'C42 H42 Cl2 N10 Ni O4 S4'
_chemical_formula_weight         1008.70
_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   mixed
_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
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2018-06-20 deposited with the CCDC.
2018-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                75.071(3)
_cell_angle_beta                 82.746(3)
_cell_angle_gamma                89.138(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1570(8)
_cell_length_b                   11.2770(9)
_cell_length_c                   18.8943(13)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      3.38
_cell_volume                     2278.2(3)
_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      172.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0522
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            83596
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.189
_diffrn_reflns_theta_min         2.930
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         10113
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      4.003
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0211P)^2^+6.1503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8582
_reflns_number_total             10113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03346c2.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
'Adding full bibliography for 7047794--7047802.cif.'
_cod_database_code               7047797
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.847
_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, All O(H) groups
2. Restrained distances
 O1S-H1S = O2S-H2S
 0.96 with sigma of 0.01
 N2-H2 = N5-H5A = N7-H7A = N10-H10A
 0.98 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(O6S) = Uiso(O5S) = Uiso(O4S)
Uiso(C6S) = Uiso(C5S) = Uiso(C4S)
4. Same fragment restrains
{O4S, C4S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O5S, C5S}
{O4S, C4S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O6S, C6S}
5. Others
 1*[Sof(O4S)+Sof(H4S)+Sof(C4S)+Sof(H4SA)+Sof(H4SB)+Sof(H4SC)]+1*[Sof(O5S)+
 Sof(H5S)+Sof(C5S)+Sof(H5SA)+Sof(H5SB)+Sof(H5SC)]+1*[Sof(O6S)+Sof(H6S)+Sof(C6S)+
 Sof(H6SA)+Sof(H6SB)+Sof(H6SC)]=1 with esd of 0
 Uiso(H2A)=Uiso(H5A)=Uiso(H7A)=Uiso(H10A)=Uiso(H2S)=Uiso(H1S)=FVAR(1)
 Sof(O4S)=Sof(H4S)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=FVAR(2)
 Sof(O5S)=Sof(H5S)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=FVAR(3)
 Sof(O6S)=Sof(H6S)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 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)
6.b Idealised Me refined as rotating group:
 C5S(H5SA,H5SB,H5SC), C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC), C6S(H6SA,H6SB,
 H6SC), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
6.c Idealised tetrahedral OH refined as rotating group:
 O5S(H5S), O3S(H3S), O6S(H6S), O4S(H4S)
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_shelx_res_checksum              62281
_olex2_submission_special_instructions 'No special instructions were received'