Adaptable 2,5-bis((1,2,3-triazol-4-yl)methoxy)pyrazine ligands for the simple self-assembly of homoleptic 1D coordination polymers
Donaldson, Marryllyn E.; Dais, Tyson N.; Rowlands, Gareth J.; Matheson, Brodie E.; Plieger, Paul G.; CrystEngComm 26 (2024) 504–516; doi:10.1039/D3CE01143G

data_7247893
_publ_section_title
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 Adaptable 2,5-bis((1,2,3-triazol-4-yl)methoxy)pyrazine ligands for the
 simple self-assembly of homoleptic 1D coordination polymers
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              504
_journal_page_last               516
_journal_paper_doi               10.1039/D3CE01143G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C26 H26 Cu N8 O2, 2(C F3 O3 S)'
_chemical_formula_sum            'C28 H26 Cu F6 N8 O8 S2'
_chemical_formula_weight         844.23
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-14 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                77.929(4)
_cell_angle_beta                 85.530(4)
_cell_angle_gamma                80.670(4)
_cell_formula_units_Z            1
_cell_length_a                   6.8471(4)
_cell_length_b                   7.8394(5)
_cell_length_c                   16.1936(9)
_cell_measurement_reflns_used    5252
_cell_measurement_temperature    100
_cell_measurement_theta_max      75.41
_cell_measurement_theta_min      2.79
_cell_volume                     837.89(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11258
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         2.793
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.4621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1883 before and 0.1074 after correction.
The Ratio of minimum to maximum transmission is 0.6129.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       needle
_exptl_crystal_F_000             429
_exptl_crystal_recrystallization_method 'Et2O into MeCN/MeOH solution'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0078(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3034
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.1185
_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^)+(0.1022P)^2^+8.9997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2791
_refine_ls_wR_factor_ref         0.2945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2325
_reflns_number_total             3034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01143g2.cif
_cod_data_source_block           DT1_4C
_cod_depositor_comments
'Adding full bibliography for 7247889--7247898.cif.'
_cod_database_code               7247893
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.649
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S6-O7 = S6-O2 = S6-O9
 1.44 with sigma of 0.02
 C2-F3 = C2-F4 = C2-F5
 1.33 with sigma of 0.02
 C2-S6
 1.82 with sigma of 0.02
 C2-O9
 2.57 with sigma of 0.04
 C2-O7
 2.58 with sigma of 0.04
 C2-O2
 2.56 with sigma of 0.04
 F3-F4 \\sim F4-F5 \\sim F5-F3
 with sigma of 0.04
 C2-F3 \\sim C2-F4 \\sim C2-F5
 with sigma of 0.02
 S6-O7 \\sim S6-O2 \\sim S6-O9
 with sigma of 0.02
 O7-O2 \\sim O2-O9 \\sim O7-O9
 with sigma of 0.04
 C2-O7 \\sim C2-O2 \\sim C2-O9
 with sigma of 0.04
 S6-F3 \\sim S6-F4 \\sim S6-F5
 with sigma of 0.04
 C2-F5 \\sim C2A-F5A
 with sigma of 0.02
 F4-S6 \\sim F4A-S6A
 with sigma of 0.04
 C2-F3 \\sim C2A-F3A
 with sigma of 0.02
 F3-F5 \\sim F3A-F5A
 with sigma of 0.04
 S6-O7 \\sim S6A-O7A
 with sigma of 0.02
 C2-F4 \\sim C2A-F4A
 with sigma of 0.02
 C2-S6 \\sim C2A-S6A
 with sigma of 0.02
 S6-O2 \\sim S6A-O1A
 with sigma of 0.02
 S6-O9 \\sim S6A-O9A
 with sigma of 0.02
 F5-S6 \\sim F5A-S6A
 with sigma of 0.04
 O7-O9 \\sim O7A-O9A
 with sigma of 0.04
 F3-S6 \\sim F3A-S6A
 with sigma of 0.04
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 O2-O9 \\sim O1A-O9A
 with sigma of 0.04
 F3-F4 \\sim F3A-F4A
 with sigma of 0.04
 O7-O2 \\sim O7A-O1A
 with sigma of 0.04
 C2-O7 \\sim C2A-O7A
 with sigma of 0.04
 C2-O2 \\sim C2A-O1A
 with sigma of 0.04
 C2-O9 \\sim C2A-O9A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 N4-C4 \\sim N4A-C4A
 with sigma of 0.04
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C3-C8 \\sim C3A-C8A
 with sigma of 0.04
 C4-C8 \\sim C4A-C8A
 with sigma of 0.02
 C6-C8 \\sim C6A-C8A
 with sigma of 0.04
 C4-C7 \\sim C4A-C7A
 with sigma of 0.04
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 N3-C5 \\sim N3-C5A
 with sigma of 0.04
 C5-C8 \\sim C5A-C8A
 with sigma of 0.04
 C3-C6 \\sim C3A-C6A
 with sigma of 0.04
 C00I-N4 \\sim C00I-N4A
 with sigma of 0.02
 C4-C9 \\sim C4A-C9A
 with sigma of 0.04
 C3-C7 \\sim C3A-C7A
 with sigma of 0.02
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 C00I-C5 \\sim C00I-C5A
 with sigma of 0.04
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C6-C9 \\sim C6A-C9A
 with sigma of 0.02
 N3-N4 \\sim N3-N4A
 with sigma of 0.02
 N4-C5 \\sim N4A-C5A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 N2-N3 \\sim N2-N3A
 with sigma of 0.02
 N3-N4 \\sim N3A-N4
 with sigma of 0.02
 N3-N4A \\sim N3A-N4A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim F3 \\sim F4 \\sim F5 \\sim S6 \\sim O7 \\sim O2 \\sim O9: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C9A) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C7A)
\\sim Ueq, Uanis(C3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim Ueq,
Uanis(C8A) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(N3A) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N3A) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) = Uanis(C2A)
Uanis(F5) = Uanis(F5A)
Uanis(F3) = Uanis(F3A)
Uanis(F4) = Uanis(F4A)
Uanis(O2) = Uanis(O1A)
Uanis(O7) = Uanis(O7A)
Uanis(O9) = Uanis(O9A)
Uanis(C9) = Uanis(C9A)
Uanis(C4) = Uanis(C4A)
Uanis(N4A) = Uanis(N4)
Uanis(C7) = Uanis(C7A)
4. Rigid body (RIGU) restrains
 C2, F3, F4, F5, S6, O7, O2, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C2(0.5) F3(0.5) F4(0.5) F5(0.5) S6(0.5) O7(0.5) O2(0.5) O9(0.5)
 S6A(0.5) O7A(0.5) O9A(0.5) O1A(0.5) F5A(0.5) F3A(0.5) F4A(0.5) C2A(0.5)
 N3(0.45) N4(0.55) C3(0.55) H3(0.55) C4(0.55) C5(0.55) H5A(0.55) H5B(0.55)
 C6(0.55) H6(0.55) C7(0.55) H7(0.55) C8(0.55) H8(0.55) C9(0.55) H9(0.55)
 N4A(0.45) C5A(0.45) H5AA(0.45) H5AB(0.45) C4A(0.45) C3A(0.45) H3A(0.45)
 C7A(0.45) H7A(0.45) C6A(0.45) H6A(0.45) C9A(0.45) H9A(0.45) C8A(0.45)
 H8A(0.45) N3A(0.55)
6.a Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B), C00D(H00D,H00E), C5(H5A,H5B), C5A(H5AA,H5AB)
6.b Aromatic/amide H refined with riding coordinates:
 C00A(H00C), C00I(H00I), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C3A(H3A),
 C7A(H7A), C6A(H6A), C9A(H9A), C8A(H8A)
;
_shelx_res_checksum              18642
_olex2_submission_special_instructions 'No special instructions were received'