Indium(iii) {2}-metallacryptates assembled from 2,6-dipicolinoyl-bis(N,N-diethylthiourea)
Pham, Chien Thang; Roca Jungfer, Maximilian; Abram, Ulrich; New Journal of Chemistry 44 (2020) 3672–3680; doi:10.1039/C9NJ06420F

data_7059312
_publ_section_title
;
 Indium(iii) {2}-metallacryptates assembled from
 2,6-dipicolinoyl-bis(N,N-diethylthiourea)
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3672
_journal_page_last               3680
_journal_paper_doi               10.1039/C9NJ06420F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C17 H25 N5 O2 S2'
_chemical_formula_sum            'C17 H25 N5 O2 S2'
_chemical_formula_weight         395.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-04 deposited with the CCDC.	2020-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.0884(15)
_cell_length_b                   38.951(4)
_cell_length_c                   12.1957(11)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      3.14
_cell_volume                     8117.6(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_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       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18325
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.740
_diffrn_reflns_theta_min         3.172
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.7086
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1110 before and 0.0970 after correction.
The Ratio of minimum to maximum transmission is 0.9148.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 1233 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3816
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.1222
_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^)+(0.0001P)^2^+240.2613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.2498
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                3471
_reflns_number_total             3816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj06420f2.cif
_cod_data_source_block           H2L
_cod_depositor_comments
;Adding full bibliography for 7059312--7059315.cif.

 Adding full bibliography for 7059312--7059315.cif.
;
_cod_database_code               7059312
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N11B-C14B
 1.5 with sigma of 0.02
 N21-C25
 1.5 with sigma of 0.02
 C26B-C25
 1.5 with sigma of 0.02
 C13B-C12B
 1.5 with sigma of 0.02
 N11B-C12B
 1.5 with sigma of 0.02
 C25A-C24 \\sim C25B-C24
 with sigma of 0.02
 N11A-C11 \\sim N11B-C11
 with sigma of 0.02
 N11B-C11 \\sim N11A-C11
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C12A) = Uanis(C12B)
Uanis(C15A) = Uanis(C14B)
Uanis(C14A) = Uanis(C15B)
Uanis(N11A) = Uanis(N11B)
Uanis(C13A) = Uanis(C13B)
Uanis(C26A) = Uanis(C26B)
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(N11B)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(C14B)=Sof(H14A)=Sof(H14B)=
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C13B)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=1-FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(N11A)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C14A)=Sof(H14C)=
 Sof(H14D)=FVAR(1)
 Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(2)
 Sof(H24A)=Sof(H24B)=Sof(C25B)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2)
 Sof(H25I)=Sof(H25J)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(3)
 Sof(H25G)=Sof(H25H)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C24(H24C,H24D), C12B(H12A,H12B), C14B(H14A,H14B), C12A(H12C,
 H12D), C14A(H14C,H14D), C25(H25G,H25H), C25(H25I,H25J)
6.b Aromatic/amide H refined with riding coordinates:
 N20(H20), N10(H10), C5(H5), C3(H3), C4(H4)
6.c Idealised Me refined as rotating group:
 C25B(H25A,H25B,H25C), C13A(H13A,H13B,H13C), C15A(H15A,H15B,H15C), C15B(H15D,
 H15E,H15F), C13B(H13D,H13E,H13F), C25A(H25D,H25E,H25F), C26A(H26A,H26B,H26C),
 C26B(H26D,H26E,H26F)
;
_shelx_res_checksum              80207
_olex2_submission_special_instructions 'No special instructions were received'