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_1572498
_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         'C68 H60 Cu10 F6 N4 O12, 2[C5H9NO]'
_chemical_formula_sum            'C78 H78 Cu10 F6 N6 O14'
_chemical_formula_weight         2072.86
_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                81.451(2)
_cell_angle_beta                 89.413(2)
_cell_angle_gamma                74.577(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6633(7)
_cell_length_b                   18.9908(12)
_cell_length_c                   20.1994(13)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      2.18
_cell_volume                     4263.0(5)
_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                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50189
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         1.629
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.516
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5398
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1278 before and 0.0771 after correction.
The Ratio of minimum to maximum transmission is 0.7245.
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    1.615
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         13997
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0721
_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^)+(0.1029P)^2^+24.3758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11163
_reflns_number_total             13997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02543a2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 1572496--1572504.cif.'
_cod_database_code               1572498
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.633
_shelx_estimated_absorpt_t_min   0.633
_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
 C2-F3
 1.29 with sigma of 0.02
 C2-F4
 1.36 with sigma of 0.02
 C2-F5
 1.27 with sigma of 0.02
 C1-F1
 1.29 with sigma of 0.02
 C1-F2
 1.36 with sigma of 0.02
 C1-F6
 1.27 with sigma of 0.02
 C2-F3 \\sim C2-F4 \\sim C2-F5
 with sigma of 0.02
 F3-F4 \\sim F4-F5 \\sim F5-F3
 with sigma of 0.03
 C1-F1 \\sim C1-F2 \\sim C1-F6
 with sigma of 0.02
 F1-F2 \\sim F2-F6 \\sim F6-F1
 with sigma of 0.03
3. Rigid bond restraints
 C01O, C02O, C02Q, C02S, C013, C00R
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C01U, C02K, C02L, C02N, C00Z, C01M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00M, O025, C02G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00H, O01Q, C020
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00M, O025, C02G, C1, F1, F2, F6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00H, O01Q, C020, C2, F3, F4, F5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C01O) \\sim Ueq, Uanis(C02O) \\sim Ueq, Uanis(C02Q) \\sim Ueq,
Uanis(C02S) \\sim Ueq, Uanis(C013) \\sim Ueq, Uanis(C00R) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C01M) \\sim Ueq, Uanis(C01U) \\sim Ueq, Uanis(C02K) \\sim Ueq,
Uanis(C02L) \\sim Ueq, Uanis(C02N) \\sim Ueq, Uanis(C00Z) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00M) \\sim Ueq, Uanis(O025) \\sim Ueq, Uanis(C02G) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00H) \\sim Ueq, Uanis(O01Q) \\sim Ueq, Uanis(C020) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00M) \\sim Ueq, Uanis(O025) \\sim Ueq, Uanis(C02G) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F6) \\sim Ueq: with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O00H) \\sim Ueq, Uanis(O01Q) \\sim Ueq, Uanis(C020) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq: with
sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00W(H00W), C00X(H00X), C00Y(H00Y), C010(H010), C011(H011),
 C014(H014), C017(H017), C01A(H01A), C01B(H01B), C01H(H01H), C01J(H01J),
 C01K(H01K), C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z),
 C021(H021), C022(H022), C023(H023), C027(H027), C028(H028), C02A(H02G)
5.b Idealised Me refined as rotating group:
 C026(H02A,H02B,H02C), C029(H02D,H02E,H02F), C02B(H02H,H02I,H02J), C02C(H02K,
 H02L,H02M), C02D(H02N,H02O,H02P), C02K(H02Q,H02R,H02S), C02L(H02T,H02U,H02V),
 C02N(H02W,H02X,H02Y), C02O(H02Z,H,HA), C02Q(H02,HB,HC), C02R(H1,HD,HE),
 C02S(H2,HF,HG)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29220
_shelx_fab_checksum              93081
_olex2_submission_special_instructions 'No special instructions were received'