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_7245556
_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
'C74 H48 Cu2 F24 N6 O10, 2(C6 H4 Cl2), 0.4(C H Cl3), 0.5(O)'
_chemical_formula_sum            'C86.4 H56.4 Cl5.2 Cu2 F24 N6 O10.5'
_chemical_formula_weight         2113.99
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-24
_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                109.391(2)
_cell_angle_beta                 92.202(2)
_cell_angle_gamma                100.595(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0105(3)
_cell_length_b                   15.1823(4)
_cell_length_c                   19.9645(3)
_cell_measurement_reflns_used    10988
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      78.0320
_cell_measurement_theta_min      3.2250
_cell_volume                     2517.69(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.96a (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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.970
_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      2.00  28.00   0.50    5.00    --  -49.87  40.00-133.00   52
  2  \w   -113.00 -37.00   0.50    5.00    --  -49.87 -40.00  72.00  152
  3  \w    -45.00  -9.00   0.50    5.00    --  -49.87  40.00-133.00   72
  4  \w     36.00 127.00   0.50    5.00    --   49.87  40.00-133.00  182
  5  \w   -165.00-135.00   0.50   20.00    --  -88.50 -40.00  72.00   60
  6  \w   -126.00-100.00   0.50   20.00    --  -88.50 -40.00  72.00   52
  7  \w     33.00 123.00   0.50   20.00    --  110.00 -40.00  72.00  180
  8  \w    107.00 169.00   0.50   20.00    --  110.00  40.00-133.00  124
  9  \w    -58.00  22.00   0.50    5.00    --  -49.87  37.00  30.00  160
 10  \w    -77.00 -40.00   0.50    5.00    --  -49.87 -57.00-150.00   74
 11  \w   -102.00 -36.00   0.50    5.00    --  -49.87 -57.00 150.00  132
 12  \w     -3.00  24.00   0.50    5.00    --   49.87 -40.00  72.00   54
 13  \w     50.00  76.00   0.50    5.00    --   49.87  57.00   0.00   52
 14  \w     26.00  71.00   0.50    5.00    --   49.87 -70.00  10.47   90
 15  \w   -108.00 -46.00   0.50   20.00    --  -88.50  70.00  61.77  124
 16  \w    -81.00 -54.00   0.50   20.00    --  -88.50  70.00 163.03   54
 17  \w   -108.00 -17.00   0.50   20.00    --  -88.50  70.00 -52.20  182
 18  \w    -82.00 -57.00   0.50   20.00    --  -88.50  40.00-133.00   50
 19  \w    -95.00 -68.00   0.50   20.00    --  -88.50  66.00 -87.71   54
 20  \w     99.00 126.00   0.50   20.00    --  110.00 -70.00 -29.23   54
 21  \w     38.00  90.00   0.50   20.00    --  110.00 -70.00  93.12  104
 22  \w    117.00 178.00   0.50   20.00    --  110.00  61.00  90.00  122
 23  \w     38.00  98.00   0.50   20.00    --  110.00 -70.00 -29.23  120
 24  \w     95.00 178.00   0.50   20.00    --  110.00  61.00  60.00  166
 25  \w    102.00 176.00   0.50   20.00    --  110.00  45.00 -60.00  148
 26  \w     50.00  94.00   0.50   20.00    --  110.00 -45.00-150.00   88
 27  \w     39.00 126.00   0.50   20.00    --  110.00 -70.00-133.17  174
 28  \w     32.00 125.00   0.50   20.00    --  110.00 -30.00 -30.00  186
 29  \w     82.00 124.00   0.50   20.00    --  110.00 -70.00 -11.96   84
 30  \w     89.00 114.00   0.50   20.00    --  110.00 -70.00 -97.16   50
 31  \w     39.00  80.00   0.50   20.00    --  110.00 -30.00  90.00   82
 32  \w    100.00 125.00   0.50   20.00    --  110.00 -30.00  90.00   50
 33  \w     79.00 121.00   0.50   20.00    --  110.00 -70.00-156.12   84
 34  \w     74.00 130.00   0.50   20.00    --  110.00 -70.00  73.50  112
 35  \w     41.00  72.00   0.50   20.00    --  110.00 -69.00 -53.33   62
 36  \w     47.00  73.00   0.50   20.00    --  110.00 -70.00-156.12   52
 37  \w     34.00  91.00   0.50   20.00    --  110.00 -30.00-180.00  114
 38  \w     62.00 115.00   0.50   20.00    --  110.00 -70.00 135.59  106
 39  \w    111.00 178.00   0.50   20.00    --  110.00  45.00-180.00  134
 40  \w    125.00 151.00   0.50   20.00    --  110.00  45.00   0.00   52
 41  \w     77.00 104.00   0.50   20.00    --  110.00 -70.00 177.04   54
 42  \w     51.00 101.00   0.50   20.00    --  110.00 -70.00  48.46  100
 43  \w     97.00 122.00   0.50   20.00    --  110.00  45.00   0.00   50
 44  \w     85.00 129.00   0.50   20.00    --  110.00 -70.00 -71.51   88
 45  \w    104.00 131.00   0.50   20.00    --  110.00 -70.00 179.62   54
 46  \w     45.00  71.00   0.50   20.00    --  110.00 -70.00 -11.96   52
 47  \w     95.00 127.00   0.50   20.00    --  110.00 -70.00  93.12   64
 48  \w     75.00 100.00   0.50   20.00    --  110.00 -70.00-116.47   50
 49  \w    138.00 171.00   0.50   20.00    --  110.00  45.00 150.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0705518000
_diffrn_orient_matrix_UB_12      -0.0869233000
_diffrn_orient_matrix_UB_13      -0.0357746000
_diffrn_orient_matrix_UB_21      -0.1280147000
_diffrn_orient_matrix_UB_22      -0.0644497000
_diffrn_orient_matrix_UB_23      0.0214765000
_diffrn_orient_matrix_UB_31      -0.0961350000
_diffrn_orient_matrix_UB_32      -0.0197254000
_diffrn_orient_matrix_UB_33      -0.0709157000
_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  0.0629
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39796
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.503
_diffrn_reflns_theta_min         3.155
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.676
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.96a (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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             1063
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.390
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         9979
_refine_ls_number_restraints     571
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0984
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2869
_refine_ls_wR_factor_ref         0.3162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6887
_reflns_number_total             9979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01130a2.cif
_cod_data_source_block           bs210528_mag199_6
_cod_original_cell_volume        2517.67(12)
_cod_original_formula_sum        'C86.40 H56.40 Cl5.20 Cu2 F24 N6 O10.50'
_cod_database_code               7245556
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H30 Cl3 Cu F12 N3 O5'
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C37B-C36B
 1.54 with sigma of 0.02
 Cl7-C48 = Cl6-C49
 1.73 with sigma of 0.02
 C48-C49 = C48-C53 = C50-C51 = C51-C52 = C52-C53
 1.38 with sigma of 0.02
 C49-C50
 1.39 with sigma of 0.02
 C28-F1
 1.3 with sigma of 0.02
 O5B-C36B
 1.2 with sigma of 0.02
 O2-C29
 1.2 with sigma of 0.02
 Cl7-C49 = Cl6-C48
 2.71 with sigma of 0.04
 C48-C52 = C50-C52
 2.39 with sigma of 0.04
 Cl6-C50
 2.69 with sigma of 0.04
 Cl7-C53
 2.67 with sigma of 0.04
 C48-C50 = C49-C51 = C51-C53
 2.4 with sigma of 0.04
 C48-Cl7 \\sim C49-Cl6
 with sigma of 0.02
 C48-C49 \\sim C49-C50 \\sim C50-C51 \\sim C51-C52 \\sim C52-C53 \\sim C53-C48
 with sigma of 0.02
 C48-C50 \\sim C48-C52 \\sim C51-C49 \\sim C51-C53 \\sim C49-C53 \\sim C50-C52
 with sigma of 0.04
 Cl7-C53 \\sim Cl7-C49 \\sim Cl6-C48 \\sim Cl6-C50
 with sigma of 0.04
 F2-F3 \\sim F3-F2B
 with sigma of 0.02
 F12B-F10B \\sim F10B-F11B
 with sigma of 0.02
3. Restrained planarity
 Cl6, Cl7, C48, C49, C50, C51, C52, C53
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Cl6 \\sim Cl7 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O5) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C33) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4B) \\sim Ueq, Uanis(C34B) \\sim Ueq, Uanis(C35B) \\sim Ueq, Uanis(C36B)
\\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(C33B) \\sim Ueq, Uanis(C37B) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 Cl1, Cl2, C41, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Cl6, Cl7, C48, C49, C50, C51, C52, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22, C23, C24, C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7B, F8B, F9B, F10B, F11B, F12B, O4B, O5B, C33B, C34B, C35B, C36B, C37B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, F8, F9, F10, F11, F12, O4, O5, C33, C34, C35, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F3, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1B, F2B, F3B, C28B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cu2(0.5) Cl1(0.5) Cl2(0.5) Cl6(0.5) Cl7(0.5) Cl3(0.2) Cl4(0.2)
 Cl5(0.2) F1B(0.5) F2B(0.5) F3B(0.5) F4B(0.5) F5B(0.5) F6B(0.5) F7B(0.5)
 F8B(0.5) F9B(0.5) F10B(0.5) F11B(0.5) F12B(0.5) F1(0.5) F2(0.5) F3(0.5)
 F4(0.5) F5(0.5) F6(0.5) F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5)
 O7(0.25) O4B(0.5) O5B(0.5) O4(0.5) O5(0.5) C45(0.5) H45(0.5) C46(0.5) H46(0.5)
 C41(0.5) C42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C28B(0.5) C29B(0.5)
 C30B(0.5) H30B(0.5) C31B(0.5) C32B(0.5) C33B(0.5) C34B(0.5) C35B(0.5)
 H35B(0.5) C36B(0.5) C37B(0.5) C48(0.5) C49(0.5) C50(0.5) H50(0.5) C51(0.5)
 H51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5) C28(0.5) C29(0.5) C30(0.5)
 H30(0.5) C31(0.5) C32(0.5) C33(0.5) C34(0.5) C35(0.5) H35(0.5) C36(0.5)
 C37(0.5) C47(0.2) H47(0.2)
7.a Ternary CH refined with riding coordinates:
 C47(H47)
7.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C45(H45), C46(H46), C43(H43), C44(H44), C30B(H30B), C35B(H35B), C50(H50),
 C51(H51), C52(H52), C53(H53), C30(H30), C35(H35)
7.d Fitted hexagon refined as free rotating group:
 C22(C23,C24,C25,C26,C27), C45(C46,C41,C42,C43,C44)
;
_shelx_res_checksum              30748
_shelx_hkl_checksum              35424
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.519
_oxdiff_exptl_absorpt_empirical_full_min 0.342