Structural diversity of copper(i) alkynyl cluster-based coordination polymers utilizing bifunctional pyridine carboxylic acid ligands
Liu, Zheng; Fang, Jun-Jie; Wang, Zhi-Yi; Xie, Yun-Peng; Lu, Xing; Nanoscale 16 (2024) 17817–17824; doi:10.1039/D4NR02543A

data_1572499
_publ_section_title
;
 Structural diversity of copper(i) alkynyl cluster-based coordination
 polymers utilizing bifunctional pyridine carboxylic acid ligands
;
_journal_issue                   38
_journal_name_full               Nanoscale
_journal_page_first              17817
_journal_page_last               17824
_journal_paper_doi               10.1039/D4NR02543A
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C70 H84 Cu13 F6 N3 O10'
_chemical_formula_sum            'C70 H84 Cu13 F6 N3 O10'
_chemical_formula_weight         2067.42
_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     iterative
_audit_creation_date             2024-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-12 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                62.883(3)
_cell_angle_beta                 80.888(3)
_cell_angle_gamma                70.396(3)
_cell_formula_units_Z            1
_cell_length_a                   13.1388(12)
_cell_length_b                   13.5488(15)
_cell_length_c                   14.2759(13)
_cell_measurement_reflns_used    2362
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      2.78
_cell_volume                     2130.8(4)
_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  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13533
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.413
_diffrn_reflns_theta_min         2.755
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.233
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5364
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0554 before and 0.0354 after correction.
The Ratio of minimum to maximum transmission is 0.7198.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.157
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.145
_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     649
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     819
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1573P)^2^+1.9761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4456
_reflns_number_total             7409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02543a2.cif
_cod_data_source_block           1d
_cod_depositor_comments
'Adding full bibliography for 1572496--1572504.cif.'
_cod_database_code               1572499
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.564
_shelx_estimated_absorpt_t_min   0.444
_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
 N50-C49 = N50-C52
 1.33 with sigma of 0.02
 C14-C15 = C15-C16
 1.54 with sigma of 0.02
 Cu5-C20
 1.86 with sigma of 0.01
 C20-C1I
 1.2 with sigma of 0.01
 C1F-C1H = C1F-C1I
 1.55 with sigma of 0.02
 Cu2-C20
 2.24 with sigma of 0.01
 Cu1-C20
 1.98 with sigma of 0.01
 C7-C8 = C8-C10
 1.54 with sigma of 0.02
 C8-C12 = C8-C13
 1.55 with sigma of 0.02
 C49-C48 = C53-C52
 1.38 with sigma of 0.02
 C48-C47 = C47-C53
 1.37 with sigma of 0.02
 C15-C17 = C15-C18
 1.55 with sigma of 0.02
 C11-F12
 1.29 with sigma of 0.02
 C11-F14
 1.36 with sigma of 0.02
 C11-F13
 1.27 with sigma of 0.02
 C2-C3 = C3-C4
 1.54 with sigma of 0.02
 C3-C5 = C3-C1
 1.55 with sigma of 0.02
 C19-C1A = C1A-C1B
 1.54 with sigma of 0.02
 C1A-C1C = C1A-C1D
 1.55 with sigma of 0.02
 C1E-C1F = C1F-C1G
 1.54 with sigma of 0.02
 C1E-C1H = C1E-C1I
 2.52 with sigma of 0.04
 C14-C16
 2.56 with sigma of 0.04
 C14-C17 = C14-C18
 2.52 with sigma of 0.04
 C7-C10
 2.56 with sigma of 0.04
 C7-C12 = C7-C13
 2.52 with sigma of 0.04
 N50-C48
 2.4 with sigma of 0.04
 N50-C53
 2.39 with sigma of 0.04
 C49-C47
 2.36 with sigma of 0.04
 C48-C53
 2.35 with sigma of 0.04
 C47-C52
 2.37 with sigma of 0.04
 C2-C4
 2.56 with sigma of 0.04
 C2-C5 = C2-C1
 2.52 with sigma of 0.04
 C19-C1B
 2.56 with sigma of 0.04
 C19-C1C = C19-C1D
 2.52 with sigma of 0.04
 C1E-C1G
 2.56 with sigma of 0.04
 C15-C16 \\sim C15-C17 \\sim C15-C18 \\sim C15-C14
 with sigma of 0.02
 C1F-C1G \\sim C1F-C1H \\sim C1F-C1I \\sim C1F-C1E
 with sigma of 0.02
 C1G-C1H \\sim C1G-C1I \\sim C1H-C1I
 with sigma of 0.04
 C14-C16 \\sim C14-C17 \\sim C14-C18
 with sigma of 0.04
 C1E-C1G \\sim C1E-C1H \\sim C1E-C1I
 with sigma of 0.04
 C16-C17 \\sim C16-C18 \\sim C17-C18
 with sigma of 0.04
 C8-C10 \\sim C8-C12 \\sim C8-C13 \\sim C8-C7
 with sigma of 0.02
 C10-C12 \\sim C10-C13 \\sim C12-C13
 with sigma of 0.04
 C7-C10 \\sim C7-C12 \\sim C7-C13
 with sigma of 0.04
 N50-C49 \\sim N50-C52
 with sigma of 0.02
 C49-C48 \\sim C48-C47 \\sim C47-C53 \\sim C53-C52
 with sigma of 0.02
 N50-C53 \\sim N50-C48
 with sigma of 0.04
 C47-C52 \\sim C47-C49 \\sim C53-C48 \\sim C52-C49
 with sigma of 0.04
 C11-F12 \\sim C11-F14 \\sim C11-F13
 with sigma of 0.02
 F12-F14 \\sim F14-F13 \\sim F13-F12
 with sigma of 0.03
 C11-F12 \\sim C11-F12A
 with sigma of 0.02
 C11-F14 \\sim C11-F14A
 with sigma of 0.02
 C11-F13 \\sim C11-F13A
 with sigma of 0.02
 C3-C4 \\sim C3-C5 \\sim C3-C1 \\sim C3-C2
 with sigma of 0.02
 C4-C5 \\sim C4-C1 \\sim C5-C1
 with sigma of 0.04
 C2-C4 \\sim C2-C5 \\sim C2-C1
 with sigma of 0.04
 C1A-C1B \\sim C1A-C1C \\sim C1A-C1D \\sim C1A-C19
 with sigma of 0.02
 C1B-C1C \\sim C1B-C1D \\sim C1C-C1D
 with sigma of 0.04
 C19-C1B \\sim C19-C1C \\sim C19-C1D
 with sigma of 0.04
3. Restrained planarity
 N50, C49, C48, C47, C53, C52
 with sigma of 0.1
4. Rigid bond restraints
 C1I, C1F, C1E, C1G, C1H, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C1I, C1F, C1E, C1G, C1H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C7, C8, C10, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8, O10, C9, C11, F12, F14, F13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32, C33, C54, C55, C57, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O46, O44, C45, N50, C49, C48, C47, C53, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C2, C3, C4, C5, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C1E \\sim C1F \\sim C1G \\sim C1H \\sim C1I: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C7 \\sim C8 \\sim C10 \\sim C12 \\sim C13: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C19 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C1E) \\sim Ueq, Uanis(C1F) \\sim Ueq, Uanis(C1G) \\sim Ueq, Uanis(C1H)
\\sim Ueq, Uanis(C1I) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O8) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F13) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C45) \\sim Ueq, Uanis(N50) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(O46) \\sim Ueq, Uanis(O44) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C6) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 C1E, C1F, C1G, C1H, C1I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C10, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N50, C49, C48, C47, C53, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C3, C4, C5, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(F14A)=Sof(F12A)=Sof(F13A)=1-FVAR(1)
 Sof(F12)=Sof(F14)=Sof(F13)=FVAR(1)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(C10)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(2)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C1A)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=
 Sof(H1BC)=Sof(C1C)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=1-FVAR(3)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C5)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(3)
 Fixed Sof: Cu1(0.5) Cu34(0.5) O46(0.5) O44(0.5) C45(0.5) Cu51(0.5) N50(0.5)
 C49(0.5) H49(0.5) C48(0.5) H48(0.5) C47(0.5) C53(0.5) H53(0.5) C52(0.5)
 H52(0.5)
8.a Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C1H(H1HA,H1HB,H1HC)
8.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C43(H43), C40(H40), C42(H42), C49(H49), C48(H48), C53(H53), C52(H52)
8.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C56(H56A,H56B,H56C), C2(H2A,H2B,
 H2C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C1B(H1BA,H1BB,
 H1BC), C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,H1EC), C1G(H1GA,H1GB,H1GC)
;
_shelx_res_checksum              35597
_shelx_fab_checksum              40445
_olex2_submission_special_instructions 'No special instructions were received'