A caged tris(2-pyridylmethyl)amine ligand equipped with a Ctriazole-H hydrogen bonding cavity.
Qiu, Gege; Diao, Donglin; Chaussy, Leo; Chevallier-Michaud, Sabine; Simaan, A. Jalila; Nava, Paola; Martinez, Alexandre; Colomban, Cedric; Dalton Transactions  (2022) –; doi:10.1039/D2DT00607C

data_7710182
_publ_section_title
;
 A caged tris(2-pyridylmethyl)amine ligand equipped with a Ctriazole-H
 hydrogen bonding cavity.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00607C
_journal_year                    2022
_chemical_formula_moiety
'3(C54 H51 Cu N13 O6), 6(C F3 O3 S), 3(C2 H3 N)'
_chemical_formula_sum            'C174 H162 Cu3 F18 N42 O36 S6'
_chemical_formula_weight         4142.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-22 deposited with the CCDC.	2022-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                87.5100(10)
_cell_angle_beta                 86.7650(10)
_cell_angle_gamma                81.9360(10)
_cell_formula_units_Z            2
_cell_length_a                   13.81820(10)
_cell_length_b                   24.6077(3)
_cell_length_c                   34.2051(4)
_cell_measurement_reflns_used    60068
_cell_measurement_temperature    203.01(10)
_cell_measurement_theta_max      70.8460
_cell_measurement_theta_min      3.2020
_cell_volume                     11490.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      203.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -1.00  24.00   1.00    5.00    --   38.00  94.00  83.41   25
  2  \w     -1.00  24.00   1.00    5.00    --   38.00  95.00-134.21   25
  3  \w   -113.00 -13.00   1.00    5.00    --  -41.32 -57.00 -60.00  100
  4  \w   -115.00 -17.00   1.00    5.00    --  -41.32 -38.00   0.00   98
  5  \w    -64.00  29.00   1.00    5.00    --  -41.32  57.00  90.00   93
  6  \w   -116.00 -17.00   1.00    5.00    --  -41.32 -38.00 120.00   99
  7  \w     23.00  90.00   1.00    5.00    --   41.32-125.00   0.00   67
  8  \w     23.00  94.00   1.00    5.00    --   41.32-125.00-120.00   71
  9  \w     11.00  37.00   1.00    5.00    --   46.00  84.00 -30.60   26
 10  \w     16.00  41.00   1.00    5.00    --   50.00  82.00  33.08   25
 11  \w     17.00  45.00   1.00    5.00    --   50.00  81.00 156.60   28
 12  \w     17.00  44.00   1.00    5.00    --   50.00  81.00  96.82   27
 13  \w     17.00  42.00   1.00    5.00    --   50.00  80.00-146.70   25
 14  \w     16.00  41.00   1.00    5.00    --   50.00  82.00 -79.59   25
 15  \w     68.00 123.00   1.00    5.00    --   58.00  77.00  61.97   55
 16  \w     26.00  51.00   1.00    5.00    --   58.00  77.00  61.97   25
 17  \w     29.00  56.00   1.00    5.00    --   62.00  77.00 154.17   27
 18  \w     33.00  59.00   1.00    5.00    --   66.00  77.00   6.74   26
 19  \w     37.00  65.00   1.00    5.00    --   70.00  77.00  84.04   28
 20  \w     38.00  64.00   1.00    5.00    --   70.00  76.00 -64.71   26
 21  \w     38.00  64.00   1.00    5.00    --   70.00  76.00-163.44   26
 22  \w     42.00  69.00   1.00   20.00    --   74.00  75.00  29.64   27
 23  \w    100.00 135.00   1.00   20.00    --   74.00  77.00 -45.22   35
 24  \w     41.00  67.00   1.00   20.00    --   74.00  77.00-154.81   26
 25  \w     41.00  70.00   1.00   20.00    --   74.00  77.00 116.77   29
 26  \w     41.00  68.00   1.00   20.00    --   74.00  77.00 -45.22   27
 27  \w     41.00  66.00   1.00   20.00    --   74.00  77.00 161.79   25
 28  \w     42.00  68.00   1.00   20.00    --   74.00  76.00-104.31   26
 29  \w     42.00  68.00   1.00   20.00    --   74.00  75.00   8.20   26
 30  \w     42.00 131.00   1.00   20.00    --   74.00  76.00  98.05   89
 31  \w     45.00  71.00   1.00   20.00    --   78.00  77.00  51.11   26
 32  \w     46.00  74.00   1.00   20.00    --   78.00  76.00-135.07   28
 33  \w     73.00 108.00   1.00   20.00    --  101.41 -94.00 -90.00   35
 34  \w     70.00 154.00   1.00   20.00    --  101.41  77.00 -90.00   84
 35  \w     99.00 170.00   1.00   20.00    --  101.41 125.00-150.00   71
 36  \w     69.00 137.00   1.00   20.00    --  101.41  77.00 150.00   68
 37  \w     69.00 124.00   1.00   20.00    --  101.41  77.00-120.00   55
 38  \w     69.00 175.00   1.00   20.00    --  101.41  77.00  90.00  106
 39  \w     99.00 151.00   1.00   20.00    --  101.41  77.00 -30.00   52
 40  \w     69.00  95.00   1.00   20.00    --  101.41  77.00 -30.00   26
 41  \w     69.00 156.00   1.00   20.00    --  101.41  77.00  60.00   87
 42  \w     69.00 155.00   1.00   20.00    --  101.41  77.00   0.00   86
 43  \w    139.00 174.00   1.00   20.00    --  101.41 125.00  90.00   35
 44  \w     69.00 165.00   1.00   20.00    --  101.41  77.00 120.00   96
 45  \w     69.00 159.00   1.00   20.00    --  101.41  77.00  30.00   90
 46  \w     69.00 177.00   1.00   20.00    --  101.41  77.00-180.00  108
 47  \w     29.00 109.00   1.00   20.00    --  101.41 -94.00 150.00   80
 48  \w     69.00 142.00   1.00   20.00    --  101.41  77.00-150.00   73
 49  \w     20.00 109.00   1.00   20.00    --  101.41 -94.00  30.00   89
 50  \w     69.00 177.00   1.00   20.00    --  101.41  77.00 -60.00  108
 51  \w     29.00 127.00   1.00   20.00    --  101.41 -61.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1076227000
_diffrn_orient_matrix_UB_12      0.0005279000
_diffrn_orient_matrix_UB_13      -0.0142827000
_diffrn_orient_matrix_UB_21      -0.0058047000
_diffrn_orient_matrix_UB_22      0.0596705000
_diffrn_orient_matrix_UB_23      0.0128085000
_diffrn_orient_matrix_UB_31      0.0331008000
_diffrn_orient_matrix_UB_32      -0.0210330000
_diffrn_orient_matrix_UB_33      0.0408604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            196803
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.189
_diffrn_reflns_theta_min         3.216
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.552
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       needle
_exptl_crystal_F_000             4266
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2611
_refine_ls_number_reflns         43691
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0936P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33344
_reflns_number_total             43691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00607c2.cif
_cod_data_source_block           cc1exp134
_cod_database_code               7710182
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'c58 h55 Cl3 Cu1 f6 n13 o12 s2'
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.637
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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. Rigid body (RIGU) restrains
 S6, F16, F17, F18, F19, F20, F21, O34, O35, O36, O37, O38, O39, C2AA, C169
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 S3, F7, F8, F9, F22, F23, F24, O25, O26, O27, C165, C170
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
3. Others
 Fixed Sof: F7(0.5) F8(0.5) F9(0.5) F22(0.5) F23(0.5) F24(0.5) C165(0.5)
 C170(0.5) F16(0.5) F17(0.5) F18(0.5) F19(0.5) F20(0.5) F21(0.5) O34(0.5)
 O35(0.5) O36(0.5) O37(0.5) O38(0.5) O39(0.5) C2AA(0.5) C169(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C10(H10A,H10B), C18(H18A,H18B), C24(H24A,H24B),
 C27(H27A,H27B), C35(H35A,H35B), C41(H41A,H41B), C44(H44A,H44B), C52(H52A,H52B),
  C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C61(H61A,H61B), C64(H64A,
 H64B), C72(H72A,H72B), C78(H78A,H78B), C81(H81A,H81B), C89(H89A,H89B),
 C95(H95A,H95B), C98(H98A,H98B), C106(H10F,H10G), C107(H10H,H10I), C108(H10J,
 H10K), C109(H10L,H10M), C115(H11A,H11B), C118(H11C,H11D), C126(H12D,H12E),
 C132(H13A,H13B), C135(H13C,H13D), C143(H14D,H14E), C149(H14F,H14G), C152(H15A,
 H15B), C160(H16A,H16B), C161(H16C,H16D), C162(H16E,H16F)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C15(H15), C20(H20), C21(H21),
 C22(H22), C25(H25), C29(H29), C32(H32), C37(H37), C38(H38), C39(H39), C43(H43),
  C46(H46), C49(H49), C57(H57), C58(H58), C59(H59), C62(H62), C66(H66),
 C69(H69), C74(H74), C75(H75), C76(H76), C79(H79), C83(H83), C86(H86), C91(H91),
  C92(H92), C93(H93), C96(H96), C100(H100), C103(H103), C111(H111), C112(H112),
 C113(H113), C116(H116), C120(H120), C123(H123), C128(H128), C129(H129),
 C130(H130), C133(H133), C137(H137), C140(H140), C145(H145), C146(H146),
 C147(H147), C150(H150), C154(H154), C157(H157)
4.c Idealised Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C51(H51A,H51B,H51C), C71(H71A,H71B,
 H71C), C88(H88A,H88B,H88C), C105(H10C,H10D,H10E), C125(H12A,H12B,H12C),
 C142(H14A,H14B,H14C), C159(H15C,H15D,H15E), C276(H27C,H27D,H27E), C270(H27F,
 H27G,H27H), C273(H27I,H27J,H27K)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 18.856
_oxdiff_exptl_absorpt_empirical_full_min 0.373