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_7245553
_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, C7 H8, 2(O)'
_chemical_formula_sum            'C81 H56 Cu2 F24 N6 O12'
_chemical_formula_weight         1888.39
_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             2021-05-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-03-29 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                100.0302(15)
_cell_angle_beta                 93.7146(16)
_cell_angle_gamma                96.8981(18)
_cell_formula_units_Z            1
_cell_length_a                   8.9300(2)
_cell_length_b                   15.7218(3)
_cell_length_c                   16.4219(3)
_cell_measurement_reflns_used    17446
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      78.6920
_cell_measurement_theta_min      2.7390
_cell_volume                     2245.21(8)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.946
_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    -63.00 -25.00   0.50    1.00    --  -49.87  57.00-150.00   76
  2  \w   -128.00 -39.00   0.50    1.00    --  -49.87 -19.00-180.00  178
  3  \w    -62.00  25.00   0.50    1.00    --  -49.87  19.00 120.00  174
  4  \w   -122.00 -39.00   0.50    1.00    --  -49.87 -57.00 -60.00  166
  5  \w     31.00 119.00   0.50    1.00    --   49.87  68.00 106.20  176
  6  \w    -21.00  70.00   0.50    1.00    --   49.87 -70.00 -21.39  182
  7  \w    -87.00 -52.00   0.50    4.00    --  -88.50  70.00 -31.42   70
  8  \w    -87.00 -58.00   0.50    4.00    --  -88.50  70.00-117.27   58
  9  \w    -93.00 -55.00   0.50    4.00    --  -88.50  70.00-146.09   76
 10  \w    -96.00 -69.00   0.50    4.00    --  -88.50  70.00  76.12   54
 11  \w     99.00 176.00   0.50    4.00    --  110.00  45.00  60.00  154
 12  \w     39.00 100.00   0.50    4.00    --  110.00 -70.00-151.90  122
 13  \w    105.00 159.00   0.50    4.00    --  110.00  45.00  30.00  108
 14  \w     33.00 124.00   0.50    4.00    --  110.00 -30.00  60.00  182
 15  \w     92.00 122.00   0.50    4.00    --  110.00 -15.00   0.00   60
 16  \w     95.00 122.00   0.50    4.00    --  110.00 -69.00 134.04   54
 17  \w    146.00 173.00   0.50    4.00    --  110.00  15.00 120.00   54
 18  \w     32.00  76.00   0.50    4.00    --  110.00 -30.00-180.00   88
 19  \w    114.00 143.00   0.50    4.00    --  110.00  15.00 120.00   58
 20  \w     54.00 107.00   0.50    4.00    --  110.00 -70.00 -87.92  106
 21  \w     92.00 118.00   0.50    4.00    --  110.00 -30.00-180.00   52
 22  \w     48.00  75.00   0.50    4.00    --  110.00 -15.00   0.00   54
 23  \w     33.00 114.00   0.50    4.00    --  110.00 -15.00  90.00  162
 24  \w    145.00 171.00   0.50    4.00    --  110.00  30.00   0.00   52
 25  \w     43.00 127.00   0.50    4.00    --  110.00 -70.00  96.32  168
 26  \w     67.00 130.00   0.50    4.00    --  110.00 -70.00  34.35  126
 27  \w     46.00 126.00   0.50    4.00    --  110.00 -70.00-131.09  160
 28  \w     79.00 106.00   0.50    4.00    --  110.00 -70.00 -37.57   54
 29  \w     48.00  93.00   0.50    4.00    --  110.00 -70.00 168.98   90
 30  \w     34.00 123.00   0.50    4.00    --  110.00 -45.00 -30.00  178
 31  \w     70.00 125.00   0.50    4.00    --  110.00 -70.00  63.50  110
 32  \w     43.00 117.00   0.50    4.00    --  110.00 -70.00  -9.53  148
 33  \w     34.00 123.00   0.50    4.00    --  110.00 -45.00-120.00  178
 34  \w    106.00 133.00   0.50    4.00    --  110.00  45.00  90.00   54
 35  \w     97.00 140.00   0.50    4.00    --  110.00  30.00   0.00   86
;
_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      0.0299165000
_diffrn_orient_matrix_UB_12      0.0987531000
_diffrn_orient_matrix_UB_13      0.0009670000
_diffrn_orient_matrix_UB_21      -0.0356114000
_diffrn_orient_matrix_UB_22      -0.0166978000
_diffrn_orient_matrix_UB_23      -0.0949271000
_diffrn_orient_matrix_UB_31      -0.1681294000
_diffrn_orient_matrix_UB_32      0.0071786000
_diffrn_orient_matrix_UB_33      0.0115793000
_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  0.0311
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29179
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.422
_diffrn_reflns_theta_min         2.743
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.675
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       prism
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.818
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         9228
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1796P)^2^+1.5075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2299
_refine_ls_wR_factor_ref         0.2463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8012
_reflns_number_total             9228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01130a2.cif
_cod_data_source_block           bs210528_mag199_2
_cod_original_cell_volume        2245.22(8)
_cod_database_code               7245553
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C90 H50 Cu2 F24 N6 O10'
_reflns_odcompleteness_completeness 97.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 C37-C36
 1.53 with sigma of 0.02
 C37B-F12B
 1.32 with sigma of 0.02
 F12-C37
 1.32 with sigma of 0.02
 C41-C42 = C41-C46 = C43-C44
 1.39 with sigma of 0.02
 C47-C41
 1.51 with sigma of 0.02
 C42-C43 = C44-C45 = C45-C46
 1.38 with sigma of 0.02
 C51-C56 = C51-C52 = C55-C54
 1.39 with sigma of 0.02
 C57-C51
 1.51 with sigma of 0.02
 C56-C55 = C54-C53 = C53-C52
 1.38 with sigma of 0.02
 C42-C44
 2.39 with sigma of 0.04
 C47-C42 = C47-C46
 2.52 with sigma of 0.04
 C41-C43
 2.42 with sigma of 0.04
 C41-C45
 2.41 with sigma of 0.04
 C43-C45 = C44-C46
 2.4 with sigma of 0.04
 C56-C54
 2.39 with sigma of 0.04
 C55-C53 = C54-C52
 2.4 with sigma of 0.04
 C51-C53
 2.41 with sigma of 0.04
 C51-C55
 2.42 with sigma of 0.04
 C57-C56 = C57-C52
 2.52 with sigma of 0.04
 F10B-F11B \\sim F11B-F12B
 with sigma of 0.02
 C41-C42 \\sim C42-C43 \\sim C43-C44 \\sim C44-C45 \\sim C45-C46 \\sim C46-C41
 with sigma of 0.02
 C41-C45 \\sim C41-C43 \\sim C46-C44 \\sim C42-C46 \\sim C43-C45 \\sim C42-C44
 with sigma of 0.04
 C47-C46 \\sim C47-C42
 with sigma of 0.04
 C51-C56 \\sim C56-C55 \\sim C55-C54 \\sim C54-C53 \\sim C53-C52 \\sim C52-C51
 with sigma of 0.02
 C51-C53 \\sim C51-C55 \\sim C52-C54 \\sim C56-C52 \\sim C55-C53 \\sim C56-C54
 with sigma of 0.04
 C57-C52 \\sim C57-C56
 with sigma of 0.04
3. Restrained planarity
 C41, C42, C43, C44, C45, C46, C47
 with sigma of 0.1
 C51, C52, C53, C54, C55, C56, C57
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 F12, C37
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F12B, C37B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C41, C42, C43, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C52, C53, C54, C55, C56, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) C33(0.5)
 C34(0.5) C35(0.5) H35(0.5) C36(0.5) C37(0.5) C51(0.25) C52(0.25) H52(0.25)
 C53(0.25) H53(0.25) C54(0.25) H54(0.25) C55(0.25) H55(0.25) C56(0.25)
 H56(0.25) C57(0.25) H57A(0.25) H57B(0.25) H57C(0.25) F7B(0.5) F8B(0.5)
 F9B(0.5) F10B(0.5) F11B(0.5) F12B(0.5) O6(0.5) O7(0.5) C33B(0.5) C34B(0.5)
 C35B(0.5) H35B(0.5) C36B(0.5) C37B(0.5) C41(0.25) C42(0.25) H42(0.25)
 C43(0.25) H43(0.25) C44(0.25) H44(0.25) C45(0.25) H45(0.25) C46(0.25)
 H46(0.25) C47(0.25) H47A(0.25) H47B(0.25) H47C(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C8(H8), 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),
  C30(H30), C35(H35), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
 C35B(H35B), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
7.c Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              15130
_shelx_hkl_checksum              65592
_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 1.687
_oxdiff_exptl_absorpt_empirical_full_min 0.670