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_1572496
_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         'C18 H22 Cu3 N O2, 0.222(C H4 O)'
_chemical_formula_sum            'C18.67 H24.67 Cu3 N O2.67'
_chemical_formula_weight         496.35
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.067(3)
_cell_length_b                   13.067(3)
_cell_length_c                   13.365(4)
_cell_measurement_reflns_used    3611
_cell_measurement_temperature    291.15
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.05
_cell_volume                     1976.3(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  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8221
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.048
_exptl_absorpt_coefficient_mu    2.410
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5581
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.7489.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2324
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0805P)^2^+5.4318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1734
_reflns_number_total             2324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02543a2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 1572496--1572504.cif.'
_cod_original_cell_volume        1976.3(11)
_cod_database_code               1572496
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.795
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(9)
 0.48(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 O3-C1
 1.4 with sigma of 0.02
 C11-C14 = C11-C13
 1.55 with sigma of 0.02
 C14A-C11 = C12A-C11 = C13A-C11
 1.54 with sigma of 0.02
 C12-C11 = C11-C10
 1.54 with sigma of 0.02
 C12-C14 = C12-C13
 2.52 with sigma of 0.04
 C12A-C13A
 2.55 with sigma of 0.04
 C12A-C14A
 2.55 with sigma of 0.04
 C12-C10
 2.56 with sigma of 0.04
 C14A-C13A
 2.55 with sigma of 0.04
 C12-C11 \\sim C12A-C11
 with sigma of 0.02
 C10-C14 \\sim C10-C13 \\sim C14-C13
 with sigma of 0.04
 C11-C10 \\sim C11-C14 \\sim C11-C13 \\sim C11-C12
 with sigma of 0.02
 C12-C10 \\sim C12-C14 \\sim C12-C13
 with sigma of 0.04
 C11-C13 \\sim C11-C13A
 with sigma of 0.02
 C11-C14 \\sim C11-C14A
 with sigma of 0.02
4. Rigid bond restraints
 C2, C11, C10, C14A, C13A, C12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9, N4, C7, C8, C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C12 \\sim C11 \\sim C10 \\sim C14 \\sim C13: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C2) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C14A)
\\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 C12, C11, C10, C14, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1)
 Fixed Sof: C1(0.333333) H1A(0.333333) H1B(0.333333) H1C(0.333333)
 O3(0.333333) H3(0.333333)
8.a Riding coordinates:
 C1(H1A,H1B,H1C)
8.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C12A(H12D,H12E,H12F)
8.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5)
8.d Tetrahedral OH refined with riding coordinates:
 O3(H3)
8.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C13A(H13D,
 H13E,H13F)
;
_shelx_res_checksum              73850
_olex2_submission_special_instructions 'No special instructions were received'