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_7059315
_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         'C51 H69 In2 N15 O6 S6, H4 N, F6 P, C7 H8'
_chemical_formula_sum            'C58 H81 F6 In2 N16 O6 P S6'
_chemical_formula_weight         1665.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-29
_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                 113.960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6320(10)
_cell_length_b                   22.5450(10)
_cell_length_c                   18.1070(10)
_cell_measurement_reflns_used    27011
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      3.36
_cell_volume                     7323.6(9)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39891
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.750
_diffrn_reflns_theta_min         3.360
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/MeOH/toluene'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00055(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         13967
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8789
_reflns_number_total             13967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj06420f2.cif
_cod_data_source_block           NH4InL
_cod_depositor_comments
;Adding full bibliography for 7059312--7059315.cif.

 Adding full bibliography for 7059312--7059315.cif.
;
_cod_original_cell_volume        7323.6(8)
_cod_database_code               7059315
_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
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H,H,H) groups
2. Restrained distances
 F1-F6
 2.2 with sigma of 0.02
 F4-F2
 2.2 with sigma of 0.02
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 F3-F6 \\sim F3A-F6A
 with sigma of 0.04
 F4-F2 \\sim F4A-F2A
 with sigma of 0.04
 F5-F2 \\sim F5A-F2A
 with sigma of 0.04
 F3-F5 \\sim F3A-F5A
 with sigma of 0.04
 F3-F2 \\sim F3A-F2A
 with sigma of 0.04
 F4-F6 \\sim F4A-F6A
 with sigma of 0.04
 F5-F6 \\sim F5A-F6A
 with sigma of 0.04
 F1-F3 \\sim F1A-F3A
 with sigma of 0.04
 F6-F2 \\sim F6A-F2A
 with sigma of 0.04
 F1-F4 \\sim F1A-F4A
 with sigma of 0.04
 F1-F5 \\sim F1A-F5A
 with sigma of 0.04
 F1-F6 \\sim F1A-F6A
 with sigma of 0.04
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F3-F4 \\sim F3A-F4A
 with sigma of 0.04
 C2_1-C6_1 \\sim C2_1-C4_1 \\sim C7_1-C5_1 \\sim C3_1-C7_1 \\sim C4_1-C6_1
\\sim C3_1-C5_1
 C2_2-C6_2 \\sim C2_2-C4_2 \\sim C7_2-C5_2 \\sim C3_2-C7_2 \\sim C4_2-C6_2
\\sim C3_2-C5_2
 with sigma of 0.04
 C2_1-C3_1 \\sim C3_1-C4_1 \\sim C4_1-C5_1 \\sim C5_1-C6_1 \\sim C6_1-C7_1
\\sim C7_1-C2_1
 C2_2-C3_2 \\sim C3_2-C4_2 \\sim C4_2-C5_2 \\sim C5_2-C6_2 \\sim C6_2-C7_2
\\sim C7_2-C2_2
 with sigma of 0.02
 C1_1-C2_1
 C1_2-C2_2
 with sigma of 0.02
 C1_1-C7_1 \\sim C1_1-C3_1
 C1_2-C7_2 \\sim C1_2-C3_2
 with sigma of 0.04
3. Restrained planarity
 C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1
 C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C52B)=Sof(H52C)=Sof(H52D)=Sof(C53B)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C1)=
 Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=1-FVAR(1)
 Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(C53A)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C1)=
 Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=FVAR(1)
 Fixed Sof: F1(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) F2(0.5) F5A(0.5) F6A(0.5)
 F3A(0.5) F2A(0.5) F4A(0.5) F1A(0.5)
6.a Riding coordinates:
 N(HB,HC)
6.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C22(H22A,H22B), C24(H24A,H24B), C42(H42A,
 H42B), C44(H44A,H44B), C54(H54A,H54B), C74(H74A,H74B), C72(H72A,H72B),
 C82(H82A,H82B), C84(H84A,H84B), C52A(H52A,H52B), C52B(H52C,H52D)
6.c Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C55(H55A,H55B,H55C), C75(H75A,
 H75B,H75C), C73(H73A,H73B,H73C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C),
 C53A(H53A,H53B,H53C), C53B(H53D,H53E,H53F)
6.d Aromatic/amide H refined with riding coordinates:
 C03(H03), C04(H04), C05(H05), C33(H33), C34(H34), C35(H35), C63(H63),
 C64(H64), C65(H65), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C3(H3), C4(H4),
 C5(H5), C6(H6), C7(H7)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              21496
_olex2_submission_special_instructions 'No special instructions were received'