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_1572502
_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         'C41 H45 Cu6 F6 N O4'
_chemical_formula_sum            'C41 H45 Cu6 F6 N O4'
_chemical_formula_weight         1111.02
_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
_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                62.3950(10)
_cell_angle_beta                 81.8880(10)
_cell_angle_gamma                64.9420(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3217(5)
_cell_length_b                   14.0632(5)
_cell_length_c                   14.6193(6)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.51
_cell_measurement_theta_min      2.75
_cell_volume                     2193.45(15)
_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 0.765
_diffrn_measured_fraction_theta_max 0.756
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.765
_diffrn_reflns_Laue_measured_fraction_max 0.756
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20313
_diffrn_reflns_point_group_measured_fraction_full 0.765
_diffrn_reflns_point_group_measured_fraction_max 0.756
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.367
_diffrn_reflns_theta_min         1.576
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.921
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6227
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1318 before and 0.0666 after correction.
The Ratio of minimum to maximum transmission is 0.8357.
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    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.0033(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         6083
_refine_ls_number_restraints     206
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0425
_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^)+(0.1045P)^2^+4.6818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5835
_reflns_number_total             6083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02543a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1572496--1572504.cif.'
_cod_database_code               1572502
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.759
_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-C3 = C3-C12
 1.54 with sigma of 0.02
 F45-C39 = F43-C39 = F40-C39
 1.35 with sigma of 0.01
 C3-C13 = C3-C14
 1.55 with sigma of 0.02
 C2-C12
 2.56 with sigma of 0.04
 C2-C13 = C2-C14
 2.52 with sigma of 0.04
 C3-C12 \\sim C3-C13 \\sim C3-C14 \\sim C3-C2
 with sigma of 0.02
 C12-C13 \\sim C12-C14 \\sim C13-C14
 with sigma of 0.04
 C2-C12 \\sim C2-C13 \\sim C2-C14
 with sigma of 0.04
3. Rigid bond restraints
 O30, O34, F36, F38, F37, C33, C32, H32, C31, C35, C39, F40, F43, F45, F42,
 F41, F44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C2, C3, C12, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C12 \\sim C13 \\sim C14: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(F40) \\sim Ueq, Uanis(F45) \\sim Ueq, Uanis(F43) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F44) \\sim Ueq, Uanis(F41) \\sim Ueq, Uanis(F42) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cu29) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C2, C3, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F42)=Sof(F41)=Sof(F44)=1-FVAR(1)
 Sof(F40)=Sof(F43)=Sof(F45)=FVAR(1)
7.a Me refined with riding coordinates:
 C59(H59A,H59B,H59C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C50(H50A,H50B,
 H50C), C19(H19A,H19B,H19C), C61(H61A,H61B,H61C), C60(H60A,H60B,H60C), C21(H21A,
 H21B,H21C), C20(H20A,H20B,H20C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C23(H23), C9(H9), C8(H8), C25(H25), C24(H24), C26(H26),
 C32(H32)
;
_shelx_res_checksum              94839
_olex2_submission_special_instructions 'No special instructions were received'