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_7059313
_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 K N15 O6 S6, F6 P, C7 H8'
_chemical_formula_sum            'C58 H77 F6 In2 K N15 O6 P S6'
_chemical_formula_weight         1686.41
_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   geom
_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                   19.6550(10)
_cell_length_b                   22.5870(10)
_cell_length_c                   18.1150(10)
_cell_measurement_reflns_used    27892
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      3.35
_cell_volume                     7349.1(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_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0879
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36307
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.749
_diffrn_reflns_theta_min         3.355
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             3440
_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         0.580
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         14004
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0428P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9456
_reflns_number_total             14004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj06420f2.cif
_cod_data_source_block           KInL
_cod_depositor_comments
;Adding full bibliography for 7059312--7059315.cif.

 Adding full bibliography for 7059312--7059315.cif.
;
_cod_original_cell_volume        7349.1(8)
_cod_database_code               7059313
_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
2. Shared sites
{C91A, C92B}
{C92A, C93B}
{C93A, C94B}
{C94A, C95B}
{C95A, C96B}
{C96A, C91B}
3. Restrained distances
 F2B-F6
 2.2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C92A) = Uanis(C92B)
Uanis(C93A) = Uanis(C93B)
Uanis(C94A) = Uanis(C94B)
Uanis(C95A) = Uanis(C95B)
Uanis(C96A) = Uanis(C96B)
5. Rigid body (RIGU) restrains
 C82B, C83B, C90B, C91B, C92B, C93B, C94B, C95B, C96B, F5, P, F3, F4, F6, F2B,
 F1, F5B, F3B, F4B, F6B, F2C, F1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C90A, C91A, C92A, C96A, C93A, C95A, C94A, C90B, C93B, C92B, C94B, C91B, C95B,
 C96B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C82B)=Sof(H82C)=Sof(H82D)=Sof(C83B)=Sof(H83D)=Sof(H83E)=Sof(H83F)=1-FVAR(1)
 Sof(C82A)=Sof(H82A)=Sof(H82B)=Sof(C83A)=Sof(H83A)=Sof(H83B)=Sof(H83C)=FVAR(1)
 Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(2)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F2C)=1-FVAR(3)
 Sof(F2B)=FVAR(3)
 Sof(F1B)=1-FVAR(4)
 Sof(F1)=FVAR(4)
 Sof(C90B)=Sof(H90D)=Sof(H90E)=Sof(H90F)=Sof(C91B)=Sof(C92B)=Sof(H92B)=
 Sof(C93B)=Sof(H93B)=Sof(C94B)=Sof(H94B)=Sof(C95B)=Sof(H95B)=Sof(C96B)=
 Sof(H96B)=1-FVAR(5)
 Sof(C90A)=Sof(H90A)=Sof(H90B)=Sof(H90C)=Sof(C91A)=Sof(C92A)=Sof(H92A)=
 Sof(C93A)=Sof(H93A)=Sof(C94A)=Sof(H94A)=Sof(C95A)=Sof(H95A)=Sof(C96A)=
 Sof(H96A)=FVAR(5)
7.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C12(H12A,H12B), C22(H22A,H22B), C24(H24A,H24B), C42(H42A,
 H42B), C44(H44A,H44B), C52(H52A,H52B), C54(H54A,H54B), C72(H72A,H72B),
 C74(H74A,H74B), C84(H84A,H84B), C82A(H82A,H82B), C82B(H82C,H82D)
7.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C53(H53A,H53B,H53C), C55(H55A,
 H55B,H55C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C85(H85A,H85B,H85C),
 C83A(H83A,H83B,H83C), C83B(H83D,H83E,H83F)
7.c 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), C92A(H92A), C93A(H93A), C94A(H94A), C95A(H95A), C96A(H96A),
  C92B(H92B), C93B(H93B), C94B(H94B), C95B(H95B), C96B(H96B)
7.d Idealised Me refined as rotating group:
 C90A(H90A,H90B,H90C), C90B(H90D,H90E,H90F)
;
_shelx_res_checksum              49862
_olex2_submission_special_instructions 'No special instructions were received'