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_1572504
_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         'C76 H84 Cu14 F12 N2 O12'
_chemical_formula_sum            'C76 H84 Cu14 F12 N2 O12'
_chemical_formula_weight         2335.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0606(8)
_cell_length_b                   23.9965(14)
_cell_length_c                   28.2045(16)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.22
_cell_volume                     8839.5(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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'ARINAX MD2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            105319
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.365
_diffrn_reflns_theta_min         1.675
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.371
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5238
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1773 before and 0.0799 after correction.
The Ratio of minimum to maximum transmission is 0.7030.
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    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.118
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         16064
_refine_ls_number_restraints     986
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0467P)^2^+106.3166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                13695
_reflns_number_total             16064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02543a2.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 1572496--1572504.cif.'
_cod_database_code               1572504
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.552
_shelx_estimated_absorpt_t_min   0.431
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(5)
 0.46(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C6-C11 = C11-C10
 1.37 with sigma of 0.02
 C71-C74 = C71-C73
 1.55 with sigma of 0.02
 C70-C71 = C71-C72
 1.54 with sigma of 0.02
 C12-C9 = C15-C14
 1.38 with sigma of 0.02
 C7-C6
 1.36 with sigma of 0.02
 C9-C8 = C8-C15
 1.37 with sigma of 0.02
 N13-C12 = N13-C14
 1.33 with sigma of 0.02
 C25-C24 = C24-C27
 1.54 with sigma of 0.02
 C24-C26 = C24-C23
 1.55 with sigma of 0.02
 C91-C90 = C90-C94
 1.54 with sigma of 0.02
 C90-C96 = C90-C89
 1.55 with sigma of 0.02
 C93-C90 = C92-C90 = C95-C90
 1.54 with sigma of 0.02
 C70-C74 = C70-C73
 2.52 with sigma of 0.04
 N13-C15
 2.39 with sigma of 0.04
 C70-C72
 2.56 with sigma of 0.04
 C7-C11 = C6-C10
 2.37 with sigma of 0.04
 C9-C15
 2.35 with sigma of 0.04
 N13-C9
 2.4 with sigma of 0.04
 C12-C8
 2.36 with sigma of 0.04
 C8-C14
 2.37 with sigma of 0.04
 C25-C27
 2.56 with sigma of 0.04
 C25-C26 = C25-C23
 2.52 with sigma of 0.04
 C91-C94
 2.56 with sigma of 0.04
 C91-C96 = C91-C89
 2.52 with sigma of 0.04
 C89-C92
 2.5 with sigma of 0.04
 C89-C93
 2.5 with sigma of 0.04
 C89-C95
 2.5 with sigma of 0.04
 C92-C95
 2.5 with sigma of 0.04
 C92-C93
 2.5 with sigma of 0.04
 C93-C95
 2.5 with sigma of 0.04
 C71-C72 \\sim C71-C74 \\sim C71-C73 \\sim C71-C70
 with sigma of 0.02
 C72-C74 \\sim C72-C73 \\sim C74-C73
 with sigma of 0.04
 C70-C72 \\sim C70-C74 \\sim C70-C73
 with sigma of 0.04
 C7-C6 \\sim C6-C11 \\sim C11-C10
 with sigma of 0.02
 C6-C10 \\sim C11-C7
 with sigma of 0.04
 C12-C9 \\sim C9-C8 \\sim C8-C15 \\sim C15-C14
 with sigma of 0.02
 N13-C15 \\sim N13-C9
 with sigma of 0.04
 C8-C14 \\sim C8-C12 \\sim C15-C9 \\sim C14-C12
 with sigma of 0.04
 N13-C12 \\sim N13-C14
 with sigma of 0.02
 C24-C27 \\sim C24-C26 \\sim C24-C23 \\sim C24-C25
 with sigma of 0.02
 C27-C26 \\sim C27-C23 \\sim C26-C23
 with sigma of 0.04
 C25-C27 \\sim C25-C26 \\sim C25-C23
 with sigma of 0.04
 C90-C94 \\sim C90-C96 \\sim C90-C89 \\sim C90-C91
 with sigma of 0.02
 C94-C96 \\sim C94-C89 \\sim C96-C89
 with sigma of 0.04
 C91-C94 \\sim C91-C96 \\sim C91-C89
 with sigma of 0.04
 C91-C90 \\sim C95-C90
 with sigma of 0.02
 C90-C94 \\sim C90-C93
 with sigma of 0.02
 C90-C96 \\sim C90-C92
 with sigma of 0.02
4. Restrained planarity
 C7, C6, C11, C10
 with sigma of 0.1
 N13, C12, C9, C8, C15, C14
 with sigma of 0.1
 C7, C6, C11, C10, N13, C12, C9, C8, C15, C14
 with sigma of 0.01
 N85, C78, C79, C80, C81, C82, C83, C104, C105, C84
 with sigma of 0.1
5. Rigid bond restraints
 C38, C70, C71, C72, C74, C73
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C6, C11, C10, N13, C12, C9, C8, C15, C14, O4, O16, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N85, C78, C104, C83, C82, C79, C105, C80, C84, C81
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C88
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19, C106, C107, C108, C109, C110
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C35, C113, C111, C112, C115, C114
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C116, C117, C118, C120, C119
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C64, C55, C66, C65, C68, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C50, C41, C51, C52, C54, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O77, N85, C76, C78, C79, C80, C81, C82, C83, O75, C104, C105, C84
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C88, C91, C90, C94, C96, C89
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C88, C90, C89, C93, C92, C95
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
C70 \\sim C71 \\sim C72 \\sim C74 \\sim C73: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C7 \\sim C6 \\sim C11 \\sim C10: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N13 \\sim C12 \\sim C9 \\sim C8 \\sim C15 \\sim C14: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C25 \\sim C24 \\sim C27 \\sim C26 \\sim C23: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C91 \\sim C90 \\sim C94 \\sim C96 \\sim C89: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C38) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(N13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N85) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C83)
\\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C80) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C81) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C88) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108)
\\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C112)
\\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C114) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C118)
\\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C119) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C64) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O77) \\sim Ueq, Uanis(N85) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(C104)
\\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C88) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C94)
\\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C89) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C88) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C95) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
7. Rigid body (RIGU) restrains
 C70, C71, C72, C74, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C6, C11, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N13, C12, C9, C8, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C24, C27, C26, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C90, C94, C96, C89
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=
 Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=1-FVAR(1)
 Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=FVAR(1)
9.a Riding coordinates:
 C66(H66A,H66B,H66C)
9.b Me refined with riding coordinates:
 C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C73(H73A,H73B,H73C)
9.c Aromatic/amide H refined with riding coordinates:
 C79(H79), C82(H82), C83(H83), C104(H104), C105(H105), C84(H84), C7(H7),
 C10(H10), C11(H11), C12(H12), C15(H15), C14(H14)
9.d Fitted hexagon refined as free rotating group:
 C78(C79,C80,C81,C82,C83), C7(C8,C9,C10,C11,C6)
9.e Idealised Me refined as rotating group:
 C113(H11A,H11B,H11C), C108(H10A,H10B,H10C), C68(H68A,H68B,H68C), C115(H11D,
 H11E,H11F), C67(H67A,H67B,H67C), C110(H11G,H11H,H11I), C118(H11J,H11K,H11L),
 C52(H52A,H52B,H52C), C120(H12A,H12B,H12C), C109(H10D,H10E,H10F), C119(H11M,
 H11N,H11O), C114(H11P,H11Q,H11R), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C),
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C91(H91A,H91B,
 H91C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C93(H93A,H93B,H93C), C92(H92A,
 H92B,H92C), C95(H95A,H95B,H95C)
;
_shelx_res_checksum              29121
_olex2_submission_special_instructions 'No special instructions were received'