Multitopic 3,2':6',3''-terpyridine ligands as 4-connecting nodes in two-dimensional 4,4-networks
Manfroni, Giacomo; Spingler, Bernhard; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; CrystEngComm  (2022) –; doi:10.1039/D2CE01130A

data_7245557
_publ_section_title
;
 Multitopic 3,2':6',3''-terpyridine ligands as 4-connecting nodes in
 two-dimensional 4,4-networks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01130A
_journal_year                    2022
_chemical_formula_moiety         'C72 H44 F24 N6 O10 Zn2, 1.8(C H Cl3), (C7 H8)'
_chemical_formula_sum            'C80.8 H53.8 Cl5.4 F24 N6 O10 Zn2'
_chemical_formula_weight         2046.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-29 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1070(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.31144(10)
_cell_length_b                   14.96748(10)
_cell_length_c                   22.80527(13)
_cell_measurement_reflns_used    46557
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      76.4330
_cell_measurement_theta_min      3.0530
_cell_volume                     4877.85(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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    -58.00  34.00   1.00    1.00    --  -40.76  37.00  60.00   92
  2  \w    -62.00  30.00   1.00    1.00    --  -40.76  37.00-180.00   92
  3  \w      2.00  33.00   1.00    1.00    --  -40.76  57.00 -90.00   31
  4  \w     22.00  64.00   1.00    1.00    --   40.76 -37.00-120.00   42
  5  \w     92.00 147.00   1.00    2.50    --  113.00  15.00   0.00   55
  6  \w     39.00 107.00   1.00    2.50    --  113.00 -45.00  60.00   68
  7  \w     92.00 141.00   1.00    2.50    --  113.00 -30.00  60.00   49
  8  \w     82.00 140.00   1.00    2.50    --  113.00  30.00-180.00   58
  9  \w    145.00 177.00   1.00    2.50    --  113.00  61.00  60.00   32
 10  \w     87.00 119.00   1.00    2.50    --  113.00 -30.00 -90.00   32
 11  \w    151.00 177.00   1.00    2.50    --  113.00  15.00   0.00   26
 12  \w     83.00 129.00   1.00    2.50    --  113.00  30.00 -60.00   46
 13  \w    134.00 162.00   1.00    2.50    --  113.00  30.00 -60.00   28
 14  \w     37.00 145.00   1.00    2.50    --  113.00 -70.00 -68.99  108
 15  \w    138.00 164.00   1.00    2.50    --  113.00  30.00  30.00   26
 16  \w     83.00 108.00   1.00    2.50    --  113.00  30.00  30.00   25
 17  \w     74.00 119.00   1.00    2.50    --  113.00 -61.00  30.00   45
 18  \w    126.00 152.00   1.00    2.50    --  113.00  61.00-180.00   26
 19  \w    115.00 140.00   1.00    2.50    --  113.00 -45.00  60.00   25
 20  \w     40.00  65.00   1.00    2.50    --  113.00 -30.00-120.00   25
 21  \w    107.00 133.00   1.00    2.50    --  113.00 -30.00-120.00   26
 22  \w     93.00 119.00   1.00    2.50    --  113.00 -67.00 -60.12   26
 23  \w     83.00 141.00   1.00    2.50    --  113.00  61.00  60.00   58
 24  \w     62.00 137.00   1.00    2.50    --  113.00 -45.00 -90.00   75
 25  \w     55.00 113.00   1.00    2.50    --  113.00  15.00  90.00   58
 26  \w    153.00 178.00   1.00    2.50    --  113.00  15.00  90.00   25
 27  \w     86.00 131.00   1.00    2.50    --  113.00  45.00 -30.00   45
 28  \w     52.00 119.00   1.00    2.50    --  113.00 -15.00  30.00   67
 29  \w     14.00 104.00   1.00    1.00    --   40.76  37.00-180.00   90
 30  \w     20.00 110.00   1.00    1.00    --   40.76  37.00  30.00   90
 31  \w      8.00  65.00   1.00    1.00    --   40.76 -19.00-180.00   57
 32  \w     85.00 117.00   1.00    2.50    --  113.00  62.00 -16.64   32
 33  \w    141.00 167.00   1.00    2.50    --  113.00  30.00-150.00   26
 34  \w     83.00 117.00   1.00    2.50    --  113.00  61.00  90.00   34
 35  \w    138.00 177.00   1.00    2.50    --  113.00  45.00 120.00   39
 36  \w     84.00 115.00   1.00    2.50    --  113.00  61.00  30.00   31
 37  \w     32.00  79.00   1.00    2.50    --  113.00 -15.00 -90.00   47
 38  \w    101.00 150.00   1.00    2.50    --  113.00 -15.00 -90.00   49
 39  \w     91.00 140.00   1.00    2.50    --  113.00  61.00-150.00   49
 40  \w    153.00 178.00   1.00    2.50    --  113.00  61.00-150.00   25
 41  \w     84.00 112.00   1.00    2.50    --  113.00  61.00 -90.00   28
 42  \w    153.00 178.00   1.00    2.50    --  113.00  61.00  90.00   25
 43  \w     56.00  82.00   1.00    2.50    --  113.00  15.00-180.00   26
 44  \w    116.00 141.00   1.00    2.50    --  113.00 -45.00 -90.00   25
 45  \w    142.00 169.00   1.00    2.50    --  113.00  15.00-180.00   27
 46  \w    100.00 138.00   1.00    2.50    --  113.00 -30.00  30.00   38
 47  \w     44.00  70.00   1.00    2.50    --  113.00 -30.00-150.00   26
 48  \w    109.00 136.00   1.00    2.50    --  113.00 -30.00-150.00   27
 49  \w     84.00 109.00   1.00    2.50    --  113.00  61.00 -30.00   25
 50  \w     90.00 115.00   1.00    2.50    --  113.00  45.00  30.00   25
 51  \w     82.00 113.00   1.00    2.50    --  113.00  30.00-120.00   31
 52  \w    125.00 151.00   1.00    2.50    --  113.00  30.00-120.00   26
 53  \w     57.00  83.00   1.00    2.50    --  113.00 -45.00 -60.00   26
 54  \w     90.00 116.00   1.00    2.50    --  113.00 -45.00 -60.00   26
 55  \w     39.00  64.00   1.00    2.50    --  113.00 -45.00 -90.00   25
 56  \w    141.00 169.00   1.00    2.50    --  113.00  61.00 -90.00   28
 57  \w     93.00 120.00   1.00    2.50    --  113.00  45.00  60.00   27
 58  \w     95.00 170.00   1.00    2.50    --  113.00  30.00 150.00   75
 59  \w     86.00 112.00   1.00    2.50    --  113.00 -70.00-106.66   26
 60  \w    123.00 149.00   1.00    2.50    --  113.00  70.00 -12.30   26
 61  \w     96.00 122.00   1.00    2.50    --  113.00  61.00   0.00   26
 62  \w    124.00 149.00   1.00    2.50    --  113.00  61.00   0.00   25
 63  \w     50.00  76.00   1.00    2.50    --  113.00 -30.00 120.00   26
 64  \w    109.00 142.00   1.00    2.50    --  113.00 -30.00 120.00   33
 65  \w     89.00 136.00   1.00    2.50    --  113.00  45.00-180.00   47
 66  \w    153.00 178.00   1.00    2.50    --  113.00  45.00 -30.00   25
 67  \w    153.00 178.00   1.00    2.50    --  113.00  30.00  30.00   25
 68  \w     60.00  86.00   1.00    2.50    --  113.00 -61.00-120.00   26
 69  \w    119.00 144.00   1.00    2.50    --  113.00 -30.00-120.00   25
 70  \w    143.00 169.00   1.00    2.50    --  113.00  15.00  90.00   26
 71  \w    140.00 171.00   1.00    2.50    --  113.00 -15.00-120.00   31
 72  \w     82.00 121.00   1.00    2.50    --  113.00  70.00 -12.30   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0616500000
_diffrn_orient_matrix_UB_12      0.0844824000
_diffrn_orient_matrix_UB_13      -0.0021503000
_diffrn_orient_matrix_UB_21      -0.0180943000
_diffrn_orient_matrix_UB_22      -0.0122033000
_diffrn_orient_matrix_UB_23      -0.0667444000
_diffrn_orient_matrix_UB_31      -0.0864782000
_diffrn_orient_matrix_UB_32      -0.0575878000
_diffrn_orient_matrix_UB_33      0.0109405000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81497
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.550
_diffrn_reflns_theta_min         3.534
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.854
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.122
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       prism
_exptl_crystal_F_000             2057
_exptl_crystal_size_max          0.613
_exptl_crystal_size_mid          0.384
_exptl_crystal_size_min          0.227
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         10223
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0797
_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/[\s^2^(Fo^2^)+(0.1736P)^2^+5.4938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2452
_refine_ls_wR_factor_ref         0.2527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9342
_reflns_number_total             10223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01130a2.cif
_cod_data_source_block           bs210531_mag185_3
_cod_original_formula_sum        'C80.80 H53.80 Cl5.40 F24 N6 O10 Zn2'
_cod_database_code               7245557
_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. Restrained distances
 C48B-C42B
 1.51 with sigma of 0.02
 C41-Cl1
 1.8 with sigma of 0.02
 C41B-Cl6B
 1.8 with sigma of 0.02
 C42B-C43B = C42B-C47B = C44B-C45B
 1.39 with sigma of 0.02
 C43B-C44B = C45B-C46B = C46B-C47B
 1.38 with sigma of 0.02
 C48B-C43B = C48B-C47B
 2.52 with sigma of 0.04
 C42B-C44B
 2.42 with sigma of 0.04
 C43B-C45B
 2.39 with sigma of 0.04
 C42B-C46B
 2.41 with sigma of 0.04
 C44B-C46B = C45B-C47B
 2.4 with sigma of 0.04
 C48B-C47B \\sim C48B-C43B
 with sigma of 0.04
 C42B-C43B \\sim C43B-C44B \\sim C44B-C45B \\sim C45B-C46B \\sim C46B-C47B
\\sim C47B-C42B
 with sigma of 0.02
 C42B-C46B \\sim C42B-C44B \\sim C47B-C45B \\sim C43B-C47B \\sim C44B-C46B
\\sim C43B-C45B
 with sigma of 0.04
3. Restrained planarity
 C42B, C43B, C44B, C45B, C46B, C47B, C48B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C42B \\sim C43B \\sim C44B \\sim C45B \\sim C46B \\sim C47B \\sim C48B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C32, F8, F9, F7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42B, C43B, C44B, C45B, C46B, C47B, C48B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20B, C21B, C22B, C23B, C24B, C25B, C26B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl4B, Cl5B, Cl6B, C41B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7B, C32, F8B, F9B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F7)=Sof(F8)=Sof(F9)=1-FVAR(1)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=FVAR(1)
 Fixed Sof: Cl4B(0.4) Cl5B(0.4) Cl6B(0.4) Cl1(0.5) Cl2(0.5) Cl3(0.5) O1(0.5)
 O1B(0.5) C41B(0.4) H41B(0.4) C7(0.5) H7(0.5) C8(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C21(0.5) C22(0.5) H22(0.5) C23(0.5)
 H23(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) C41(0.5)
 H41(0.5) C7B(0.5) H7B(0.5) C8B(0.5) C19B(0.5) H19C(0.5) H19D(0.5) C20B(0.5)
 H20C(0.5) H20D(0.5) C21B(0.5) C22B(0.5) H22B(0.5) C23B(0.5) H23B(0.5)
 C24B(0.5) H24B(0.5) C25B(0.5) H25B(0.5) C26B(0.5) H26B(0.5) C42B(0.5)
 C43B(0.5) H43B(0.5) C44B(0.5) H44B(0.5) C45B(0.5) H45B(0.5) C46B(0.5)
 H46B(0.5) C47B(0.5) H47B(0.5) C48B(0.25) H48A(0.25) H48B(0.25) H48C(0.25)
7.a Ternary CH refined with riding coordinates:
 C41B(H41B), C41(H41)
7.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C19B(H19C,H19D), C20B(H20C,H20D)
7.c Me refined with riding coordinates:
 C48B(H48A,H48B,H48C)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C29(H29), C34(H34), C7(H7), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C7B(H7B), C22B(H22B), C23B(H23B), C24B(H24B), C25B(H25B),
 C26B(H26B), C43B(H43B), C44B(H44B), C45B(H45B), C46B(H46B), C47B(H47B)
7.e Fitted hexagon refined as free rotating group:
 C21(C22,C23,C24,C25,C26)
;
_shelx_res_checksum              91353
_shelx_hkl_checksum              65360
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.863