#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:12:17 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229280 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/77/7047794.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7047794
loop_
_publ_author_name
'Pringouri, Konstantina'
'Anwar, Muhammad U.'
'Mansour, Liz'
'Doupnik, Nathan'
'Beldjoudi, Yassine'
'Gavey, Emma L.'
'Pilkington, Melanie'
'Rawson, Jeremy M.'
_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(C F3 O3 S), C38 H26 Mn N10 S4'
_chemical_formula_sum            'C40 H26 F6 Mn N10 O6 S6'
_chemical_formula_weight         1104.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-30
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7882(7)
_cell_length_b                   19.1313(9)
_cell_length_c                   14.6344(8)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.85
_cell_volume                     4420.3(4)
_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      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65724
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         2.852
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0584 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.9451.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       plate
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4530
_refine_ls_number_restraints     429
_refine_ls_restrained_S_all      1.394
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0412
_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/[σ²(Fo²)+(0.0406P)²+9.5317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3532
_reflns_number_total             4530
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03346c2.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
'Adding full bibliography for 7047794--7047802.cif.'
_cod_database_code               7047794
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F3A-F1A \\sim F3A-F2A \\sim F1A-F2A
 with sigma of 0.04
 C20-S3 \\sim C20-F1 \\sim C20-F2 \\sim C20-F3 \\sim C20-F3A \\sim C20-F1A
\\sim C20-F2A
 with sigma of 0.02
 O1-O2 \\sim O1-O3 \\sim O2-O3 \\sim O3A-O1A \\sim O3A-O2A \\sim O1A-O2A
 with sigma of 0.04
 S3-O1 \\sim S3-O2 \\sim S3-O3 \\sim S3-O3A \\sim S3-O1A \\sim S3-O2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
Uanis(O1) = Uanis(O1A)
Uanis(O2) = Uanis(O2A)
Uanis(O3) = Uanis(O3A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F3A)=Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=1-FVAR(2)
 Sof(O1)=Sof(O2)=Sof(O3)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N2(H2), C11(H11), C10(H10), C9(H9), C2(H2A), C15(H15), C16(H16),
 C4(H4), C18(H18), C3(H3), C17(H17), C5(H5A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.72284(18) 0.64244(19) 0.6617(2) 0.0541(9) Uani 0.881(4) 1 d D U . A 1
O2 O 0.60999(18) 0.57182(12) 0.72128(19) 0.0380(7) Uani 0.881(4) 1 d D U . A 1
O3 O 0.5769(2) 0.66776(16) 0.6213(2) 0.0550(10) Uani 0.881(4) 1 d D U . A 1
O1A O 0.7099(10) 0.6021(12) 0.6865(18) 0.0541(9) Uani 0.119(4) 1 d D U . A 2
O2A O 0.5585(10) 0.5913(8) 0.6798(14) 0.0380(7) Uani 0.119(4) 1 d D U . A 2
O3A O 0.6209(17) 0.6842(11) 0.6015(14) 0.0550(10) Uani 0.119(4) 1 d D U . A 2
Mn1 Mn 0.2500 0.7500 0.37424(4) 0.01598(14) Uani 1 2 d S TU P . .
S1 S 0.32791(4) 0.87243(4) 0.53268(5) 0.02601(18) Uani 1 1 d . U . . .
S3 S 0.63476(5) 0.63881(4) 0.68414(5) 0.02745(18) Uani 1 1 d D U . . .
S2 S 0.12703(4) 0.64083(4) 0.23666(6) 0.02669(18) Uani 1 1 d . U . . .
N3 N 0.35911(13) 0.67893(11) 0.38573(15) 0.0157(4) Uani 1 1 d . U . . .
N4 N 0.22663(13) 0.65777(11) 0.27933(16) 0.0185(5) Uani 1 1 d . U . . .
N5 N 0.26865(14) 0.54085(11) 0.25329(15) 0.0199(5) Uani 1 1 d . U . . .
H5 H 0.2947 0.5058 0.2803 0.024 Uiso 1 1 calc R . . . .
N1 N 0.34977(14) 0.79992(12) 0.46802(15) 0.0189(5) Uani 1 1 d . U . . .
N2 N 0.47865(15) 0.78052(12) 0.54631(16) 0.0235(5) Uani 1 1 d . U . . .
H2 H 0.5095 0.7468 0.5700 0.028 Uiso 1 1 calc R . . . .
C7 C 0.41749(16) 0.76383(13) 0.48518(18) 0.0171(5) Uani 1 1 d . U . . .
C12 C 0.36228(16) 0.62330(14) 0.32988(17) 0.0165(5) Uani 1 1 d . U . . .
C13 C 0.28019(16) 0.60695(13) 0.28535(18) 0.0161(5) Uani 1 1 d . U . . .
C8 C 0.42973(16) 0.70021(13) 0.42807(18) 0.0168(5) Uani 1 1 d . U . . .
C14 C 0.21542(16) 0.52743(14) 0.17709(18) 0.0179(5) Uani 1 1 d . U . . .
C1 C 0.43074(17) 0.89983(14) 0.56652(18) 0.0197(6) Uani 1 1 d . U . . .
C6 C 0.49480(17) 0.85023(14) 0.57345(19) 0.0212(6) Uani 1 1 d . U . . .
C11 C 0.43739(17) 0.58807(14) 0.31283(19) 0.0208(6) Uani 1 1 d . U . . .
H11 H 0.4385 0.5487 0.2733 0.025 Uiso 1 1 calc R . . . .
C10 C 0.51053(17) 0.61141(15) 0.35438(19) 0.0210(6) Uani 1 1 d . U . . .
H10 H 0.5630 0.5890 0.3421 0.025 Uiso 1 1 calc R . . . .
C9 C 0.50751(16) 0.66772(14) 0.41410(18) 0.0186(5) Uani 1 1 d . U . . .
H9 H 0.5571 0.6836 0.4445 0.022 Uiso 1 1 calc R . . . .
C2 C 0.44703(19) 0.96914(15) 0.58845(19) 0.0242(6) Uani 1 1 d . U . . .
H2A H 0.4042 1.0035 0.5809 0.029 Uiso 1 1 calc R . . . .
C19 C 0.14814(17) 0.57230(14) 0.15883(19) 0.0200(6) Uani 1 1 d . U . . .
C15 C 0.23334(17) 0.47210(15) 0.11909(19) 0.0225(6) Uani 1 1 d . U . . .
H15 H 0.2789 0.4413 0.1324 0.027 Uiso 1 1 calc R . . . .
C16 C 0.18416(19) 0.46194(16) 0.0411(2) 0.0281(6) Uani 1 1 d . U . . .
H16 H 0.1964 0.4244 0.0008 0.034 Uiso 1 1 calc R . . . .
C4 C 0.58979(19) 0.93863(16) 0.6286(2) 0.0292(7) Uani 1 1 d . U . . .
H4 H 0.6439 0.9519 0.6510 0.035 Uiso 1 1 calc R . . . .
C18 C 0.09948(19) 0.56221(16) 0.0810(2) 0.0291(7) Uani 1 1 d . U . . .
H18 H 0.0540 0.5931 0.0676 0.035 Uiso 1 1 calc R . . . .
C3 C 0.52641(19) 0.98791(16) 0.6215(2) 0.0280(6) Uani 1 1 d . U . . .
H3 H 0.5370 1.0349 0.6392 0.034 Uiso 1 1 calc R . . . .
C17 C 0.1174(2) 0.50669(17) 0.0225(2) 0.0316(7) Uani 1 1 d . U . . .
H17 H 0.0837 0.4995 -0.0304 0.038 Uiso 1 1 calc R . . . .
C5 C 0.57491(19) 0.86962(16) 0.6032(2) 0.0273(6) Uani 1 1 d . U . . .
H5A H 0.6192 0.8361 0.6061 0.033 Uiso 1 1 calc R . . . .
C20 C 0.6248(2) 0.69618(17) 0.7808(2) 0.0385(8) Uani 1 1 d D U . . .
F1 F 0.6405(2) 0.76222(14) 0.7627(3) 0.0479(8) Uani 0.799(3) 1 d D U . B 1
F2 F 0.6830(2) 0.68033(14) 0.84880(18) 0.0532(8) Uani 0.799(3) 1 d D U . B 1
F3 F 0.55163(19) 0.69020(18) 0.8242(2) 0.0656(10) Uani 0.799(3) 1 d D U . B 1
F3A F 0.6131(8) 0.6640(6) 0.8556(7) 0.0656(10) Uani 0.201(3) 1 d D U . B 2
F1A F 0.5389(6) 0.7272(5) 0.7629(8) 0.0479(8) Uani 0.201(3) 1 d D U . B 2
F2A F 0.6697(9) 0.7531(7) 0.7726(11) 0.0532(8) Uani 0.201(3) 1 d D U . B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N3 Mn1 N3 171.23(12) 2_565 .
N3 Mn1 N4 72.22(8) . .
N3 Mn1 N4 113.50(8) . 2_565
N3 Mn1 N4 113.50(8) 2_565 .
N3 Mn1 N4 72.22(8) 2_565 2_565
N3 Mn1 N1 103.55(8) . 2_565
N3 Mn1 N1 71.00(8) . .
N3 Mn1 N1 103.55(8) 2_565 .
N3 Mn1 N1 71.00(8) 2_565 2_565
N4 Mn1 N4 104.77(12) . 2_565
N4 Mn1 N1 142.96(8) 2_565 2_565
N4 Mn1 N1 86.05(8) . 2_565
N4 Mn1 N1 86.05(8) 2_565 .
N4 Mn1 N1 142.96(8) . .
N1 Mn1 N1 106.62(12) 2_565 .
N1 S1 C1 102.05(12) . .
O1 S3 O2 113.09(19) . .
O1 S3 C20 103.66(17) . .
O2 S3 C20 102.81(16) . .
O3 S3 O1 117.4(2) . .
O3 S3 O2 114.72(19) . .
O3 S3 C20 102.55(18) . .
O1A S3 O2A 112.4(11) . .
O1A S3 O3A 116.0(14) . .
O1A S3 C20 111.5(10) . .
O2A S3 C20 109.3(8) . .
O3A S3 O2A 101.4(11) . .
O3A S3 C20 105.5(10) . .
N4 S2 C19 101.59(12) . .
C12 N3 Mn1 118.18(16) . .
C8 N3 Mn1 119.95(17) . .
C8 N3 C12 119.5(2) . .
S2 N4 Mn1 121.00(11) . .
C13 N4 Mn1 115.84(17) . .
C13 N4 S2 118.74(19) . .
C13 N5 C14 121.2(2) . .
S1 N1 Mn1 121.88(11) . .
C7 N1 Mn1 117.36(17) . .
C7 N1 S1 119.32(19) . .
C7 N2 C6 122.4(2) . .
N1 C7 N2 126.2(2) . .
N1 C7 C8 115.7(2) . .
N2 C7 C8 118.1(2) . .
N3 C12 C13 113.7(2) . .
N3 C12 C11 121.8(2) . .
C11 C12 C13 124.4(2) . .
N4 C13 N5 126.0(2) . .
N4 C13 C12 116.3(2) . .
N5 C13 C12 117.7(2) . .
N3 C8 C7 113.6(2) . .
N3 C8 C9 122.1(2) . .
C9 C8 C7 124.2(2) . .
C19 C14 N5 119.4(2) . .
C15 C14 N5 119.9(2) . .
C15 C14 C19 120.6(2) . .
C6 C1 S1 118.9(2) . .
C2 C1 S1 121.0(2) . .
C2 C1 C6 120.0(3) . .
C1 C6 N2 119.5(2) . .
C5 C6 N2 120.3(3) . .
C5 C6 C1 120.2(3) . .
C10 C11 C12 118.6(2) . .
C11 C10 C9 120.0(2) . .
C10 C9 C8 118.0(2) . .
C1 C2 C3 119.6(3) . .
C14 C19 S2 118.5(2) . .
C18 C19 S2 121.8(2) . .
C18 C19 C14 119.6(3) . .
C14 C15 C16 119.6(3) . .
C17 C16 C15 119.9(3) . .
C3 C4 C5 120.4(3) . .
C19 C18 C17 119.9(3) . .
C4 C3 C2 120.3(3) . .
C16 C17 C18 120.3(3) . .
C6 C5 C4 119.4(3) . .
F1 C20 S3 114.3(3) . .
F1 C20 F2 103.3(3) . .
F1 C20 F3 110.2(3) . .
F2 C20 S3 111.9(2) . .
F3 C20 S3 113.6(2) . .
F3 C20 F2 102.4(3) . .
F3A C20 S3 113.3(6) . .
F3A C20 F1A 102.1(8) . .
F3A C20 F2A 124.2(9) . .
F1A C20 S3 100.5(4) . .
F2A C20 S3 113.0(8) . .
F2A C20 F1A 98.3(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 S3 1.430(3) .
O2 S3 1.446(3) .
O3 S3 1.410(3) .
O1A S3 1.378(13) .
O2A S3 1.510(12) .
O3A S3 1.504(13) .
Mn1 N3 2.201(2) 2_565
Mn1 N3 2.201(2) .
Mn1 N4 2.276(2) 2_565
Mn1 N4 2.276(2) .
Mn1 N1 2.297(2) 2_565
Mn1 N1 2.297(2) .
S1 N1 1.714(2) .
S1 C1 1.776(3) .
S3 C20 1.797(3) .
S2 N4 1.723(2) .
S2 C19 1.768(3) .
N3 C12 1.343(3) .
N3 C8 1.339(3) .
N4 C13 1.292(3) .
N5 C13 1.361(3) .
N5 C14 1.420(3) .
N1 C7 1.297(3) .
N2 C7 1.355(3) .
N2 C6 1.415(4) .
C7 C8 1.489(4) .
C12 C13 1.484(4) .
C12 C11 1.387(4) .
C8 C9 1.391(4) .
C14 C19 1.392(4) .
C14 C15 1.386(4) .
C1 C6 1.391(4) .
C1 C2 1.388(4) .
C6 C5 1.388(4) .
C11 C10 1.379(4) .
C10 C9 1.388(4) .
C2 C3 1.390(4) .
C19 C18 1.387(4) .
C15 C16 1.394(4) .
C16 C17 1.385(4) .
C4 C3 1.379(4) .
C4 C5 1.392(4) .
C18 C17 1.393(5) .
C20 F1 1.314(4) .
C20 F2 1.388(4) .
C20 F3 1.323(4) .
C20 F3A 1.269(10) .
C20 F1A 1.503(9) .
C20 F2A 1.304(11) .
