Isostructural coordination polymers of the tethering naphthalene anchored bis(2-methylpyridinecarboxamide) ligand: single crystal, XPS, EDS and theoretical studies
Rana, Love Karan; Kaur, Prabhjyot; Bavandsavadkouhi, Alborz; Selopal, Gurpreet Singh; Duong, Adam; New Journal of Chemistry 47 (2023) 5477–5487; doi:10.1039/D3NJ00038A

data_7062350
_publ_section_title
;
 Isostructural coordination polymers of the tethering naphthalene anchored
 bis(2-methylpyridinecarboxamide) ligand: single crystal, XPS, EDS and
 theoretical studies
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5477
_journal_page_last               5487
_journal_paper_doi               10.1039/D3NJ00038A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C36 H48 Cu N8 O6, 2(Cl O4)'
_chemical_formula_sum            'C36 H48 Cl2 Cu N8 O14'
_chemical_formula_weight         951.26
_chemical_name_systematic        Cu-26N4
_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             2022-11-03
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-25 deposited with the CCDC.	2023-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                95.500(7)
_cell_angle_beta                 107.674(8)
_cell_angle_gamma                100.676(7)
_cell_formula_units_Z            1
_cell_length_a                   9.2489(8)
_cell_length_b                   10.8769(8)
_cell_length_c                   11.2251(10)
_cell_measurement_reflns_used    3043
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.9240
_cell_measurement_theta_min      4.1440
_cell_volume                     1043.27(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0715
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_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    -54.00 -23.00   1.00    7.26    --  -36.47  61.00   6.00   31
  2  \w    -93.00 -46.00   1.00    7.26    --  -36.47 -61.00-132.00   47
  3  \w      5.00  30.00   1.00    7.26    --  -36.47  61.00   6.00   25
  4  \w     24.00  50.00   1.00    7.26    --   36.47  61.00   6.00   26
  5  \w    103.00 175.00   1.00    7.00    --  107.77  61.00   6.00   72
  6  \w     47.00 114.00   1.00    7.00    --  107.77 -61.00-132.00   67
  7  \w   -103.00 -21.00   1.00    7.26    --  -36.47 -57.00 150.00   82
  8  \w     33.00 104.00   1.00    7.26    --   36.47  57.00  30.00   71
  9  \w     30.00  89.00   1.00    7.26    --   36.47-125.00-120.00   59
 10  \w     27.00 101.00   1.00    7.26    --   36.47  57.00 -60.00   74
 11  \w     50.00  85.00   1.00    7.26    --   36.47-125.00 120.00   35
 12  \w     -2.00  25.00   1.00    7.26    --   36.47 -61.00-132.00   27
 13  \w    -21.00  44.00   1.00    7.26    --   36.47 -77.00  90.00   65
 14  \w     39.00 119.00   1.00    7.00    --  107.77 -45.00 -60.00   80
 15  \w     45.00 105.00   1.00    7.00    --  107.77-111.00 -90.00   60
 16  \w    116.00 155.00   1.00    7.00    --  107.77 111.00 -60.00   39
 17  \w     65.00 102.00   1.00    7.00    --  107.77 -94.00 -30.00   37
 18  \w    116.00 172.00   1.00    7.00    --  107.77 111.00 -30.00   56
 19  \w     69.00 105.00   1.00    7.00    --  107.77 -94.00  30.00   36
 20  \w     38.00 103.00   1.00    7.00    --  107.77-111.00 150.00   65
 21  \w     45.00 102.00   1.00    7.00    --  107.77 -94.00 150.00   57
 22  \w     91.00 146.00   1.00    7.00    --  107.77 -15.00-180.00   55
 23  \w    109.00 147.00   1.00    7.00    --  107.77  77.00-150.00   38
 24  \w     45.00  71.00   1.00    7.00    --  107.77 -15.00-180.00   26
 25  \w     99.00 173.00   1.00    7.00    --  107.77  61.00 -90.00   74
 26  \w    107.00 133.00   1.00    7.00    --  107.77  77.00 -30.00   26
 27  \w     64.00 120.00   1.00    7.00    --  107.77 178.00-180.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Definition file'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0155823000
_diffrn_orient_matrix_UB_12      0.0474332000
_diffrn_orient_matrix_UB_13      -0.1273205000
_diffrn_orient_matrix_UB_21      0.0943978000
_diffrn_orient_matrix_UB_22      -0.0932973000
_diffrn_orient_matrix_UB_23      -0.0322903000
_diffrn_orient_matrix_UB_31      -0.1518331000
_diffrn_orient_matrix_UB_32      -0.1018936000
_diffrn_orient_matrix_UB_33      -0.0636961000
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7014
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.451
_diffrn_reflns_theta_min         4.189
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plates
_exptl_crystal_F_000             495
_exptl_crystal_preparation       'Vapor diffusion ethylacetate/DMF'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0831P)^2^+0.5995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3284
_reflns_number_total             4000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00038a2.cif
_cod_data_source_block           cu-26n4
_cod_depositor_comments
'Adding full bibliography for 7062349--7062352.cif.'
_cod_database_code               7062350
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.699
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3A-C18A \\sim N3A-C18
 with sigma of 0.02
 N3A-C17A \\sim N3A-C17
 with sigma of 0.02
 N4A-C13A \\sim N4-C13
 with sigma of 0.02
 N3A-C16A \\sim N3A-C16
 with sigma of 0.02
 O6A-C16A \\sim O6A-C16
 with sigma of 0.02
 C15A-C13A \\sim C15-C13
 with sigma of 0.04
 N4A-C15A \\sim N4-C15
 with sigma of 0.02
 C13A-C14A \\sim C13-C14
 with sigma of 0.04
 N4A-C14A \\sim N4-C14
 with sigma of 0.02
 C15A-C14A \\sim C15-C14
 with sigma of 0.04
 Cl1-O4 \\sim Cl1-O4A
 with sigma of 0.02
 Cl1-O1 \\sim Cl1-O1A
 with sigma of 0.02
 Cl1-O2 \\sim Cl1-O2A
 with sigma of 0.02
 Cl1-O3 \\sim Cl1-O3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C14)
Uanis(C13A) = Uanis(C13)
Uanis(C18) = Uanis(C18A)
4. Rigid body (RIGU) restrains
 O7A, O7, C13, C13A, N4A, N4, C15, C15A, C14, C14A, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O1, O2, O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O1, O2, O3, O4, O2A, O3A, O4A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7A, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=Sof(N4)=Sof(O7)=1-FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(N4A)=Sof(O7A)=FVAR(1)
 Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=
 Sof(H18B)=Sof(H18C)=Sof(N3)=Sof(O6)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(N3A)=Sof(O6A)=FVAR(2)
 Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O1A)=1-FVAR(3)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C13A(H13A), C16(H16), C16A(H16A), N2(H2)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C14A(H14D,H14E,H14F), C15A(H15D,
 H15E,H15F), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C17A(H17D,H17E,H17F),
 C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              62028
_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 1.119
_oxdiff_exptl_absorpt_empirical_full_min 0.885