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_7062349
_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 Co N8 O6, 2(Cl O4)'
_chemical_formula_sum            'C36 H48 Cl2 Co N8 O14'
_chemical_formula_weight         946.65
_chemical_name_systematic        Co-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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-17
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6197)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2023-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                95.171(5)
_cell_angle_beta                 105.936(5)
_cell_angle_gamma                103.407(6)
_cell_formula_units_Z            1
_cell_length_a                   9.1612(6)
_cell_length_b                   10.9721(8)
_cell_length_c                   11.5145(4)
_cell_measurement_reflns_used    4172
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.7130
_cell_measurement_theta_min      4.0430
_cell_volume                     1067.87(12)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0715
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_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    -37.00  -8.00   1.00    5.34    --  -36.47  -6.00 -52.00   29
  2  \w     12.00  37.00   1.00    5.34    --   36.47  -6.00 -52.00   25
  3  \w    -32.00 106.00   1.00    5.34    --   36.47   6.00 123.00  138
  4  \w     94.00 134.00   1.00   21.34    --  107.77  -6.00 -52.00   40
  5  \w     40.00  91.00   1.00   21.34    --  107.77  -6.00 -52.00   51
  6  \w    128.00 153.00   1.00   21.34    --  107.77   6.00 123.00   25
  7  \w   -101.00 -55.00   1.00    5.34    --  -36.47   6.00 123.00   46
  8  \w    -52.00 -27.00   1.00    5.34    --  -36.47  38.00 150.00   25
  9  \w    -25.00  33.00   1.00    5.34    --  -36.47  38.00 150.00   58
 10  \w    -45.00 -10.00   1.00    5.34    --  -36.47 125.00 -90.00   35
 11  \w      7.00  60.00   1.00    5.34    --   36.47 -99.00 -60.00   53
 12  \w     29.00  89.00   1.00    5.34    --   36.47-125.00-150.00   60
 13  \w      1.00  27.00   1.00    5.34    --   36.47 -77.00  90.00   26
 14  \w      7.00  44.00   1.00    5.34    --   36.47 -99.00-120.00   37
 15  \w     28.00  83.00   1.00    5.34    --   36.47-125.00  60.00   55
 16  \w     46.00 105.00   1.00   21.34    --  107.77 -94.00  90.00   59
 17  \w     59.00 106.00   1.00   21.34    --  107.77 -94.00-180.00   47
 18  \w     40.00 121.00   1.00   21.34    --  107.77 -45.00-180.00   81
 19  \w     40.00 108.00   1.00   21.34    --  107.77-111.00   0.00   68
 20  \w     39.00 128.00   1.00   21.34    --  107.77 -30.00   0.00   89
 21  \w     61.00  86.00   1.00   21.34    --  107.77 -61.00  60.00   25
 22  \w    105.00 151.00   1.00   21.34    --  107.77  77.00 120.00   46
 23  \w    100.00 125.00   1.00   21.34    --  107.77 -30.00-180.00   25
 24  \w    103.00 131.00   1.00   21.34    --  107.77  77.00 -30.00   28
 25  \w     54.00  86.00   1.00   21.34    --  107.77 -30.00-180.00   32
 26  \w     81.00 106.00   1.00   21.34    --  107.77 -94.00   0.00   25
 27  \w    104.00 172.00   1.00   21.34    --  107.77  77.00 150.00   68
 28  \w     50.00 125.00   1.00   21.34    --  107.77 -45.00  90.00   75
 29  \w     63.00 121.00   1.00   21.34    --  107.77 -61.00 -60.00   58
 30  \w     56.00  83.00   1.00   21.34    --  107.77 -94.00-150.00   27
 31  \w     60.00  95.00   1.00   21.34    --  107.77-111.00 -60.00   35
;
_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      0.1705017000
_diffrn_orient_matrix_UB_12      -0.0005432000
_diffrn_orient_matrix_UB_13      0.0080571000
_diffrn_orient_matrix_UB_21      -0.0404951000
_diffrn_orient_matrix_UB_22      -0.1432723000
_diffrn_orient_matrix_UB_23      0.0055187000
_diffrn_orient_matrix_UB_31      -0.0473211000
_diffrn_orient_matrix_UB_32      -0.0297685000
_diffrn_orient_matrix_UB_33      -0.1407227000
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7666
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.405
_diffrn_reflns_theta_min         4.048
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60350
_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 pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plates
_exptl_crystal_F_000             493
_exptl_crystal_preparation       'Vapour diffusion technique'
_exptl_crystal_recrystallization_method 'DMF/ EtOH'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0735P)^2^+0.1959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3812
_reflns_number_total             4109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00038a2.cif
_cod_data_source_block           co-26n4
_cod_depositor_comments
'Adding full bibliography for 7062349--7062352.cif.'
_cod_database_code               7062349
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.71
_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), C16(H16), C9(H9), C4(H4), C11(H11), C1(H1), C2(H2A), C12(H12), C5(H5),
  C13(H13)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C)
;
_shelx_res_checksum              69619
_olex2_exptl_crystal_mounting_method
;
X-ray crystallographic data for the crystal was collected by mounting the crystal on a loop fiber. Data were collected 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 crystal-to-detector distance 
was 4.0 cm.
;
_olex2_submission_original_sample_id Co-26N4
_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 1.730
_oxdiff_exptl_absorpt_empirical_full_min 0.709