Substituents Make a Difference: 6,6’’-modified Terpyridine Complexes with Helix Configuration and Enhanced Emission
Fu, Fan; Liu, Die; Zhao, Lili; Li, Huili; Bai, Xinyu; Chen, Mingzhao; Jiang, Zhilong; Su, Peiyang; Zhong, Wanying; Li, Yiming; Liao, Wei-Ming; He, Jun; Wang, Pingshan; Dalton Transactions  (2023) –; doi:10.1039/D2DT04006A

data_7712224
_publ_section_title
;
 Substituents Make a Difference: 6,6&#x2019;&#x2019;-modified Terpyridine
 Complexes with Helix Configuration and Enhanced Emission
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT04006A
_journal_year                    2023
_chemical_formula_moiety         'C70 H54 Co N6 O4, 2(F6 P)'
_chemical_formula_sum            'C70 H54 Co F12 N6 O4 P2'
_chemical_formula_weight         1392.06
_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
_audit_creation_date             2022-10-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-16 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.614(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2116(5)
_cell_length_b                   24.5320(6)
_cell_length_c                   15.6483(4)
_cell_measurement_reflns_used    43545
_cell_measurement_temperature    99.99(11)
_cell_measurement_theta_max      30.7640
_cell_measurement_theta_min      2.2520
_cell_volume                     6733.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -9.00  67.00   0.50   36.48    --    4.52  57.00 -30.00  152
  2  \w     -8.00  79.00   0.50   36.48    --    4.52  19.00 120.00  174
  3  \w    -20.00  36.00   0.50   36.48    --   -6.00  33.00  79.31  112
  4  \w    -20.00  57.00   0.50   36.48    --   -6.00  33.00 -78.26  154
  5  \w    -20.00  56.00   0.50   36.48    --   -6.00  33.00 -15.35  152
  6  \w     43.00  68.00   0.50   36.48    --   -6.00  33.00  79.31   50
  7  \w    -17.00  27.00   0.50   36.48    --   -6.24 -99.00-180.00   88
  8  \w    -18.00  27.00   0.50   36.48    --   -6.24 -99.00 120.00   90
  9  \w    -19.00  39.00   0.50   36.48    --   -6.24  28.00  49.09  116
 10  \w    -19.00  69.00   0.50   36.48    --   -6.24  30.00 170.01  176
 11  \w    -16.00  26.00   0.50   36.48    --   -6.24 -99.00  60.00   84
 12  \w    -19.00  65.00   0.50   36.48    --   -6.24  28.00-139.31  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0106265000
_diffrn_orient_matrix_UB_12      -0.0264967000
_diffrn_orient_matrix_UB_13      -0.0102508000
_diffrn_orient_matrix_UB_21      0.0103232000
_diffrn_orient_matrix_UB_22      0.0109177000
_diffrn_orient_matrix_UB_23      -0.0327055000
_diffrn_orient_matrix_UB_31      0.0446721000
_diffrn_orient_matrix_UB_32      0.0038399000
_diffrn_orient_matrix_UB_33      0.0214536000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            167204
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.255
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       needle
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         15455
_refine_ls_number_restraints     659
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.1031
_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^)+(0.0128P)^2^+37.6649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13242
_reflns_number_total             15455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04006a2.cif
_cod_data_source_block           ff167-2
_cod_database_code               7712224
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O00X-C04M \\sim O00Y-C04M
 with sigma of 0.02
 C047-C04M \\sim C1-C04M
 with sigma of 0.04
 O00X-C047 \\sim O00Y-C1
 with sigma of 0.02
3. Restrained planarity
 C12, C13, C17, C11, C03Q, C10, C02M
 with sigma of 0.1
 C03F, C055, C05F, C03W, C03P, C03Q, C02M
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F00L \\sim P006 \\sim F1 \\sim F0 \\sim F00P \\sim F02M \\sim F03L: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C05F \\sim C03W \\sim C03P \\sim C03F \\sim C055 \\sim C12 \\sim C03Q \\sim C13
\\sim C17 \\sim C10 \\sim C11: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O057 \\sim O0 \\sim C04D \\sim C040 \\sim C05J \\sim C052 \\sim C020 \\sim C01P
\\sim C04N \\sim C2 \\sim C3 \\sim C5 \\sim C6 \\sim C7 \\sim C0 \\sim C05K:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O00X \\sim C047 \\sim C04M: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 C12, C13, C17, C11, C03Q, C10, C02M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C03W, C055, C03F, C03Q, C05F, C03P, C02M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C040, C05J, C052, C020, C01P, C04N, C2, C5, C6, C05K, O057, O0, C04D, C3, C7,
 C0, C03G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C04M
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C047, O00X, C04M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C17)=Sof(H17)=Sof(C10)=Sof(H10)=
 Sof(C11)=Sof(H11)=1-FVAR(1)
 Sof(C05F)=Sof(H05F)=Sof(C03W)=Sof(H03W)=Sof(C03P)=Sof(H03P)=Sof(C03F)=
 Sof(H03F)=Sof(C055)=Sof(H055)=FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(O00Y)=1-FVAR(2)
 Sof(O00X)=Sof(C047)=Sof(H04A)=Sof(H04B)=Sof(H04C)=FVAR(2)
 Fixed Sof: O057(0.612) O0(0.388) C04D(0.612) H04E(0.612) C040(0.612)
 C05J(0.612) H05J(0.612) C052(0.612) H052(0.612) C020(0.612) C01P(0.612)
 H01P(0.612) C04N(0.612) H04F(0.612) H04H(0.612) H04K(0.612) C2(0.388)
 H2(0.388) C3(0.388) H3(0.388) C5(0.388) H5(0.388) C6(0.388) C7(0.388)
 H7A(0.388) H7B(0.388) H7C(0.388) C0(0.388) C05K(0.388) H05K(0.388)
7.a Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00U(H00U), C010(H010), C01J(H01J), C01U(H01U), C028(H028),
 C02H(H02H), C02K(H02K), C02N(H02N), C02U(H02U), C04Y(H04Y), C04G(H04G),
 C024(H024), C02O(H02O), C02Q(H02Q), C02R(H02R), C03I(H03I), C03J(H03J),
 C03L(H03L), C03M(H03M), C03S(H03S), C03V(H03V), C042(H042), C046(H046),
 C048(H048), C04A(H04D), C04D(H04E), C05J(H05J), C052(H052), C01P(H01P),
 C04I(H04I), C04J(H04J), C04V(H04V), C04W(H04W), C04X(H04X), C056(H056),
 C05B(H05B), C05F(H05F), C03W(H03W), C03P(H03P), C03F(H03F), C055(H055), C2(H2),
  C3(H3), C5(H5), C05K(H05K), C12(H12), C13(H13), C17(H17), C10(H10), C11(H11)
7.b Fitted hexagon refined as free rotating group:
 C12(C03Q,C13,C17,C10,C11)
7.c Idealised Me refined as rotating group:
 C03Y(H03A,H03B,H03C), C047(H04A,H04B,H04C), C04N(H04F,H04H,H04K), C05E(H05A,
 H05C,H05D), C7(H7A,H7B,H7C), C1(H1A,H1B,H1C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              59310
_shelx_fab_checksum              89738
_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 1.698
_oxdiff_exptl_absorpt_empirical_full_min 0.689