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_1572503
_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         '1.993(C32 H40 Cu6 F3 N O4), C6 H10'
_chemical_formula_sum            'C69.76 H90 Cu12 F6 N2 O8'
_chemical_formula_weight         1961.06
_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
_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                90
_cell_angle_beta                 94.883(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.310(3)
_cell_length_b                   18.0920(19)
_cell_length_c                   18.612(2)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.51
_cell_measurement_theta_min      2.21
_cell_volume                     8156.2(16)
_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      273.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            95455
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.362
_diffrn_reflns_theta_min         0.841
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.3778
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1623 before and 0.0875 after correction.
The Ratio of minimum to maximum transmission is 0.5070.
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    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             3954
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.952
_refine_diff_density_min         -1.926
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         14105
_refine_ls_number_restraints     1013
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1384P)^2^+16.5636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.1952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12288
_reflns_number_total             14105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02543a2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 1572496--1572504.cif.'
_cod_original_cell_volume        8155.9(17)
_cod_database_code               1572503
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.455
_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
 C89-F92
 1.36 with sigma of 0.02
 C99-C102 = C99-C101
 1.55 with sigma of 0.02
 C98-C99 = C99-C100
 1.54 with sigma of 0.02
 C106-C105 = C105-C108
 1.54 with sigma of 0.02
 C105-C107 = C105-C104
 1.55 with sigma of 0.02
 C89-F90
 1.29 with sigma of 0.02
 C89-F91
 1.27 with sigma of 0.02
 C77-C78
 1.54 with sigma of 0.02
 C77-C80 = C77-C79
 1.55 with sigma of 0.02
 C76-C81 = C81-C82
 1.54 with sigma of 0.02
 C81-C84 = C81-C83
 1.55 with sigma of 0.02
 C98-C102 = C98-C101
 2.52 with sigma of 0.04
 C98-C100
 2.56 with sigma of 0.04
 C106-C108
 2.56 with sigma of 0.04
 C106-C107 = C106-C104
 2.52 with sigma of 0.04
 C76-C82
 2.56 with sigma of 0.04
 C76-C84 = C76-C83
 2.52 with sigma of 0.04
 C99-C100 \\sim C99-C102 \\sim C99-C101 \\sim C99-C98
 with sigma of 0.02
 C89-F90 \\sim C89-F92 \\sim C89-F91
 with sigma of 0.02
 F90-F92 \\sim F92-F91 \\sim F91-F90
 with sigma of 0.03
 C100-C102 \\sim C100-C101 \\sim C102-C101
 with sigma of 0.04
 C98-C100 \\sim C98-C102 \\sim C98-C101
 with sigma of 0.04
 C105-C108 \\sim C105-C107 \\sim C105-C104 \\sim C105-C106
 with sigma of 0.02
 C108-C107 \\sim C108-C104 \\sim C107-C104
 with sigma of 0.04
 C106-C108 \\sim C106-C107 \\sim C106-C104
 with sigma of 0.04
 C77-C78 \\sim C77-C80 \\sim C77-C79
 with sigma of 0.02
 C78-C80 \\sim C78-C79 \\sim C80-C79
 with sigma of 0.04
 C81-C82 \\sim C81-C84 \\sim C81-C83 \\sim C81-C76
 with sigma of 0.02
 C82-C84 \\sim C82-C83 \\sim C84-C83
 with sigma of 0.04
 C76-C82 \\sim C76-C84 \\sim C76-C83
 with sigma of 0.04
3. Rigid bond restraints
 C89, F90, F92, F91
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C75
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C70, C69, C73, C71, C72, C74
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C48, C93, C49, C94, C96, C95
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C85, C86, C88, C87, C55, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C13, C14, C15, C17, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C42, C43, C44, C46, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C22, C23, C24, C26, C25, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C98, C99, C100, C102, C101, C97
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C104, C106, C105, C108, C107, C103
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N64, C62, C61, C63, C65, C66, O59, O67, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O51, O53, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8, F19, O10, F21, F20, C9, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C75, C77, C78, C80, C79, C76, C81, C82, C84, C83
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu5, Cu1, Cu3, Cu4, Cu7, Cu11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu54, Cu57, Cu68, Cu58, Cu47, Cu50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C98 \\sim C99 \\sim C100 \\sim C102 \\sim C101: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C106 \\sim C105 \\sim C108 \\sim C107 \\sim C104: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C77 \\sim C78 \\sim C80 \\sim C79: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C76 \\sim C81 \\sim C82 \\sim C84 \\sim C83: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C89) \\sim Ueq, Uanis(F90) \\sim Ueq, Uanis(F92) \\sim Ueq, Uanis(F91)
\\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C75) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C70) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C48) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C94)
\\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C95) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C88)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C2) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C98) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C102)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C97) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C106) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C108) \\sim Ueq,
Uanis(C107) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C103) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(N64) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(O59) \\sim Ueq,
Uanis(O67) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O51) \\sim Ueq, Uanis(O53) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O8) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(F21)
\\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C18) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C75) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C83) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(Cu7) \\sim Ueq, Uanis(Cu11) \\sim Ueq, Uanis(Cu5) \\sim Ueq, Uanis(Cu1)
\\sim Ueq, Uanis(Cu3) \\sim Ueq, Uanis(Cu4) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(Cu57) \\sim Ueq, Uanis(Cu68) \\sim Ueq, Uanis(Cu47) \\sim Ueq,
Uanis(Cu58) \\sim Ueq, Uanis(Cu50) \\sim Ueq, Uanis(Cu54) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cu58) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 C98, C99, C100, C102, C101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C106, C105, C108, C107, C104
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C77, C78, C80, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C76, C81, C82, C84, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C81)=Sof(C82)=Sof(H82a)=Sof(H82b)=Sof(H82c)=Sof(C84)=Sof(H84a)=Sof(H84b)=
 Sof(H84c)=Sof(C83)=Sof(H83a)=Sof(H83b)=Sof(H83c)=1-FVAR(1)
 Sof(C77)=Sof(C78)=Sof(H78a)=Sof(H78b)=Sof(H78c)=Sof(C80)=Sof(H80a)=Sof(H80b)=
 Sof(H80c)=Sof(C79)=Sof(H79a)=Sof(H79b)=Sof(H79c)=Sof(C76)=FVAR(1)
 Fixed Sof: C106(0.5) H10a(0.5) H10b(0.5) H10c(0.5) C105(0.5) C108(0.5)
 H10d(0.5) H10e(0.5) H10f(0.5) C107(0.5) H10g(0.5) H10h(0.5) H10i(0.5)
 C104(0.5) C103(0.5) H103(0.5) C98(0.5) C99(0.5) C100(0.5) H10j(0.5) H10k(0.5)
 H10l(0.5) C102(0.5) H10m(0.5) H10n(0.5) H10o(0.5) C101(0.5) H10p(0.5)
 H10q(0.5) H10r(0.5) C97(0.5) H97(0.5)
7.a Me refined with riding coordinates:
 C100(H10j,H10k,H10l), C102(H10m,H10n,H10o)
7.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C38(H38), C62(H62), C63(H63), C40(H40), C65(H65), C41(H41), C66(H66)
7.c Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C73(H73a,H73b,H73c), C25(H25a,H25b,
 H25c), C30(H30a,H30b,H30c), C32(H32a,H32b,H32c), C72(H72a,H72b,H72c), C94(H94a,
 H94b,H94c), C96(H96a,H96b,H96c), C44(H44a,H44b,H44c), C74(H74a,H74b,H74c),
 C95(H95a,H95b,H95c), C15(H15a,H15b,H15c), C46(H46a,H46b,H46c), C31(H31a,H31b,
 H31c), C17(H17a,H17b,H17c), C45(H45a,H45b,H45c), C86(H86a,H86b,H86c), C88(H88a,
 H88b,H88c), C16(H16a,H16b,H16c), C87(H87a,H87b,H87c), C106(H10a,H10b,H10c),
 C108(H10d,H10e,H10f), C107(H10g,H10h,H10i), C101(H10p,H10q,H10r), C78(H78a,
 H78b,H78c), C80(H80a,H80b,H80c), C79(H79a,H79b,H79c), C82(H82a,H82b,H82c),
 C84(H84a,H84b,H84c), C83(H83a,H83b,H83c)
7.d :
 C103(H103), C97(H97)
;
_shelx_res_checksum              68697
_olex2_submission_special_instructions 'No special instructions were received'