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_1572501
_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         'C78.184 H88 Cu12.504 F7.662 N2 O9.907'
_chemical_formula_sum            'C78.19 H88 Cu12.5 F7.66 N2 O9.91'
_chemical_formula_weight         2154.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 108.4950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8539(2)
_cell_length_b                   15.62430(10)
_cell_length_c                   24.1728(2)
_cell_measurement_reflns_used    36892
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.9940
_cell_measurement_theta_min      3.4350
_cell_volume                     8543.90(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     40.00  82.00   0.50    0.50    --    0.00  46.00  21.29   84
  2  \w    -33.00  23.00   0.50    0.50    --    0.00 -82.00  60.00  112
  3  \w    -32.00  20.00   0.50    0.50    --    0.00 -82.00 -60.00  104
  4  \w     -9.00  20.00   0.50    0.50    --    0.00 -82.00-120.00   58
  5  \w    -31.00  28.00   0.50    0.50    --    0.00 -82.00-150.00  118
  6  \w    -33.00  27.00   0.50    0.50    --    0.00 -82.00   0.00  120
  7  \w    -19.00  28.00   0.50    0.50    --    0.00  46.00  21.29   94
  8  \w     56.00  82.00   0.50    0.50    --   95.20 -77.00  30.00   52
  9  \w      6.00  33.00   0.50    0.50    --   95.20 -77.00  30.00   54
 10  \w    111.00 168.00   0.50    0.50    --   95.20  61.00 -30.00  114
 11  \w     19.00 119.00   0.50    0.50    --   95.20 -61.00 -60.00  200
 12  \w     42.00 101.00   0.50    0.50    --   95.20 -82.00  90.00  118
 13  \w     92.00 118.00   0.50    0.50    --   95.20 -82.00  60.00   52
 14  \w     72.00 132.00   0.50    0.50    --   95.20  15.00  30.00  120
 15  \w      6.00 118.00   0.50    0.50    --   95.20 -15.00   0.00  224
 16  \w     15.00 118.00   0.50    0.50    --   95.20 -61.00-180.00  206
 17  \w     23.00 127.00   0.50    0.50    --   95.20 -82.00 -60.00  208
 18  \w    147.00 185.00   0.50    0.50    --   95.20  15.00 -60.00   76
 19  \w     77.00 102.00   0.50    0.50    --   95.20 -82.00  30.00   50
 20  \w     75.00 138.00   0.50    0.50    --   95.20  15.00 -60.00  126
 21  \w     16.00  42.00   0.50    0.50    --   95.20 -82.00 -90.00   52
 22  \w     74.00 100.00   0.50    0.50    --   95.20 -82.00 -90.00   52
 23  \w     26.00 109.00   0.50    0.50    --   95.20 -30.00  30.00  166
 24  \w    144.00 184.00   0.50    0.50    --   95.20  15.00  30.00   80
 25  \w     13.00  38.00   0.50    0.50    --   95.20 -82.00   0.00   50
 26  \w     94.00 125.00   0.50    0.50    --   95.20 -82.00   0.00   62
 27  \w    100.00 125.00   0.50    0.50    --   95.20 -77.00  30.00   50
 28  \w     69.00 102.00   0.50    0.50    --   95.20 -82.00 120.00   66
 29  \w     20.00 118.00   0.50    0.50    --   95.20 -82.00-180.00  196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0665251000
_diffrn_orient_matrix_UB_12      -0.0194705000
_diffrn_orient_matrix_UB_13      -0.0259187000
_diffrn_orient_matrix_UB_21      0.0025609000
_diffrn_orient_matrix_UB_22      0.0208801000
_diffrn_orient_matrix_UB_23      -0.0614415000
_diffrn_orient_matrix_UB_31      0.0142797000
_diffrn_orient_matrix_UB_32      -0.0943802000
_diffrn_orient_matrix_UB_33      -0.0082848000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48339
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.517
_diffrn_reflns_theta_min         3.438
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       block
_exptl_crystal_F_000             4328
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.000151(13)
_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   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         8599
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0732P)^2^+36.6602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8265
_reflns_number_total             8599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02543a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1572496--1572504.cif.'
_cod_original_formula_sum        'C78.19 H88 Cu12.50 F7.66 N2 O9.91'
_cod_database_code               1572501
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.594
_shelx_estimated_absorpt_t_min   0.345
_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
 O1-C2 = O4-C2
 1.25 with sigma of 0.01
 C5-O1
 2.35 with sigma of 0.01
 O4-C5
 2.35 with sigma of 0.01
 O1-O4
 2.25 with sigma of 0.01
 F2-F00N
 2.15 with sigma of 0.04
 F00E-F00N
 2.15 with sigma of 0.04
 F2-F00E
 2.15 with sigma of 0.04
 F00M-F00L
 2.15 with sigma of 0.04
 F00M-F00D
 2.15 with sigma of 0.04
 F00D-F00L
 2.15 with sigma of 0.04
 F00D-C015 \\sim F00E-C015
 with sigma of 0.02
 F00L-C015 \\sim F2-C015
 with sigma of 0.02
 F00M-C015 \\sim F00N-C015
 with sigma of 0.02
 C00F-C00P \\sim C00F-C4
 with sigma of 0.02
 C00P-C01C \\sim C4-C3
 with sigma of 0.02
 C01C-C01F \\sim C3-C01G
 with sigma of 0.02
 C01C-C01H \\sim C3-C1
 with sigma of 0.02
 C01C-C01I \\sim C3-C01J
 with sigma of 0.02
 C00F-C01C \\sim C00F-C3
 with sigma of 0.04
 C00P-C01F \\sim C4-C01G
 with sigma of 0.04
 C00P-C01H \\sim C4-C1
 with sigma of 0.04
 C00P-C01I \\sim C4-C01J
 with sigma of 0.04
 C01F-C01H \\sim C01G-C1
 with sigma of 0.04
 C01F-C01I \\sim C01G-C01J
 with sigma of 0.04
 C01H-C01I \\sim C1-C01J
 with sigma of 0.04
3. Restrained planarity
 O4, C2, O1, C5
 with sigma of 0.001
4. Rigid bond restraints
 O4, C2, O1, C5, F3, F1, F4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O008, F00D, F00L, F00M, C00Q, C015, O00B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O4, F1, C2, F3, F4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00P, C01C, C01F, C01H, C01I, C00F
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00O, C012, C01B, C01D, C01E, C00G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00F, C00P, C01C, C01F, C01H, C01I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00F, C01J, C1, C3, C01G, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O008) \\sim Ueq, Uanis(O00B) \\sim Ueq, Uanis(F00D) \\sim Ueq,
Uanis(F00L) \\sim Ueq, Uanis(F00M) \\sim Ueq, Uanis(C00Q) \\sim Ueq,
Uanis(C015) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C00G) \\sim Ueq, Uanis(C00O) \\sim Ueq, Uanis(C012) \\sim Ueq,
Uanis(C01B) \\sim Ueq, Uanis(C01D) \\sim Ueq, Uanis(C01E) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00F) \\sim Ueq, Uanis(C00P) \\sim Ueq, Uanis(C01C) \\sim Ueq,
Uanis(C01F) \\sim Ueq, Uanis(C01H) \\sim Ueq, Uanis(C01I) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00F) \\sim Ueq, Uanis(C01J) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C01G) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C01H) \\sim Ueq, Uanis(C01F) \\sim Ueq, Uanis(C00P) \\sim Ueq,
Uanis(C01C) \\sim Ueq, Uanis(C01I) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
6. Others
 Sof(F00N)=Sof(F2)=Sof(F00E)=1-FVAR(1)
 Sof(F00D)=Sof(F00L)=Sof(F00M)=FVAR(1)
 Sof(C01J)=Sof(H2)=Sof(HH)=Sof(HI)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C3)=
 Sof(C01G)=Sof(H3)=Sof(HJ)=Sof(HK)=Sof(C4)=1-FVAR(2)
 Sof(C00P)=Sof(C01C)=Sof(C01F)=Sof(H01Z)=Sof(HB)=Sof(HC)=Sof(C01H)=Sof(H01)=
 Sof(HD)=Sof(HE)=Sof(C01I)=Sof(H1)=Sof(HF)=Sof(HG)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00R(H00R), C00U(H00U), C00W(H00W), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C014(H014)
7.b Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C016(H01D,H01E,H01F), C017(H01G,H01H,H01I), C018(H01J,
 H01K,H01L), C019(H01M,H01N,H01O), C01A(H01P,H01Q,H01R), C01B(H01S,H01T,H01U),
 C01D(H01V,H01W,H01X), C01E(H01Y,H,HA), C01F(H01Z,HB,HC), C01H(H01,HD,HE),
 C01I(H1,HF,HG), C01J(H2,HH,HI), C1(H1A,H1B,H1C), C01G(H3,HJ,HK)
;
_shelx_res_checksum              53520
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.474
_oxdiff_exptl_absorpt_empirical_full_min 0.644