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_7062352
_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 N8 O6 Zn, 2(Cl O4)'
_chemical_formula_sum            'C36 H48 Cl2 N8 O14 Zn'
_chemical_formula_weight         953.09
_chemical_name_systematic        Zn-26N3
_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     dual
_audit_creation_date             2021-02-16
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-16 deposited with the CCDC.	2023-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                95.177(4)
_cell_angle_beta                 106.101(4)
_cell_angle_gamma                103.357(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1957(4)
_cell_length_b                   10.9757(6)
_cell_length_c                   11.4963(4)
_cell_measurement_reflns_used    4105
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.7300
_cell_measurement_theta_min      4.1710
_cell_volume                     1069.76(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.965
_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    -41.00  11.00   1.00   15.00    --  -36.60  35.00  -8.00   52
  2  \w   -106.00 -19.00   1.00   15.00    --  -36.60 -35.00-165.00   87
  3  \w    -13.00  12.00   1.00   15.00    --   36.60 -35.00-165.00   25
  4  \w     18.00  93.00   1.00   15.00    --   36.60  35.00  -8.00   75
  5  \w    103.00 177.00   1.00   22.00    --  107.46  35.00  -8.00   74
  6  \w     59.00 127.00   1.00   22.00    --  107.46 -35.00-165.00   68
  7  \w    -55.00  32.00   1.00   15.00    --  -36.60  38.00 120.00   87
  8  \w     24.00  59.00   1.00   15.00    --   36.60  57.00-150.00   35
  9  \w    -21.00  46.00   1.00   15.00    --   36.60 -77.00   0.00   67
 10  \w     40.00  90.00   1.00   15.00    --   36.60-125.00 -60.00   50
 11  \w     22.00  51.00   1.00   15.00    --   36.60  57.00-180.00   29
 12  \w     38.00  70.00   1.00   15.00    --   36.60 -99.00  90.00   32
 13  \w     96.00 129.00   1.00   22.00    --  107.46 -30.00   0.00   33
 14  \w     39.00  86.00   1.00   22.00    --  107.46 -30.00  90.00   47
 15  \w     65.00 144.00   1.00   22.00    --  107.46 -15.00 -30.00   79
 16  \w     50.00 104.00   1.00   22.00    --  107.46-111.00 150.00   54
 17  \w     44.00 107.00   1.00   22.00    --  107.46 -94.00 -60.00   63
 18  \w     52.00  78.00   1.00   22.00    --  107.46 -30.00   0.00   26
 19  \w    128.00 175.00   1.00   22.00    --  107.46 111.00   0.00   47
 20  \w     77.00 109.00   1.00   22.00    --  107.46-111.00-120.00   32
 21  \w     37.00  63.00   1.00   22.00    --  107.46-111.00-120.00   26
 22  \w     39.00 115.00   1.00   22.00    --  107.46 -45.00 -60.00   76
 23  \w     45.00  80.00   1.00   22.00    --  107.46 -94.00-180.00   35
 24  \w     71.00 109.00   1.00   22.00    --  107.46-111.00  30.00   38
 25  \w    126.00 156.00   1.00   22.00    --  107.46  77.00 120.00   30
 26  \w    102.00 171.00   1.00   22.00    --  107.46  61.00  30.00   69
 27  \w     77.00 128.00   1.00   22.00    --  107.46 -77.00   0.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0426441000
_diffrn_orient_matrix_UB_12      -0.1434619000
_diffrn_orient_matrix_UB_13      0.0040501000
_diffrn_orient_matrix_UB_21      -0.1741661000
_diffrn_orient_matrix_UB_22      -0.0093281000
_diffrn_orient_matrix_UB_23      -0.0639045000
_diffrn_orient_matrix_UB_31      0.0244456000
_diffrn_orient_matrix_UB_32      -0.0269604000
_diffrn_orient_matrix_UB_33      -0.1260875000
_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  0.0235
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7064
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.866
_diffrn_reflns_theta_min         4.058
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_preparation       'Vapour diffusion'
_exptl_crystal_recrystallization_method DMF/EtOH
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0543P)^2^+0.6202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3543
_reflns_number_total             4059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00038a2.cif
_cod_data_source_block           l5-zn_auto
_cod_depositor_comments
'Adding full bibliography for 7062349--7062352.cif.'
_cod_database_code               7062352
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H18 N4 O6 Cl2 Zn'
_reflns_odcompleteness_completeness 99.26
_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.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C17(H17), C11(H11), C9(H9), C4(H4), C2(H2A), C12(H12), C5(H5), C1(H1),
  C13(H13)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C15(H15A,H15B,
 H15C)
;
_shelx_res_checksum              86179
_olex2_exptl_crystal_mounting_method
'Single crystal was mounted on a loop fiber and the X-ray data  using a Rigaku New Gemini, Dual, four circle diffractometer equipped with a EosS2 Detector, graphite monochromator and a fine-focus sealed X-ray tube. The Cu K\a radiations were used for the analysis and the crystal-to-detector distance'
_olex2_submission_original_sample_id Zn-26N3
_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 3.190
_oxdiff_exptl_absorpt_empirical_full_min 0.746