Aqueous syntheses of anthracene-based mixed-ligand coordination polymers and their structural and optical properties
Marttinen, Antti; Lahtinen, Manu; CrystEngComm 26 (2024) 3388–3400; doi:10.1039/D4CE00399C

data_7248792
_publ_section_title
;
 Aqueous syntheses of anthracene-based mixed-ligand coordination polymers
 and their structural and optical properties
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              3388
_journal_page_last               3400
_journal_paper_doi               10.1039/D4CE00399C
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C116 H80 N20 Ni3 O16 S2, 12[H2O], 4[C3H7NO]'
_chemical_formula_sum            'C128 H132 N24 Ni3 O32 S2'
_chemical_formula_weight         2758.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.823(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5935(3)
_cell_length_b                   29.6842(9)
_cell_length_c                   17.6639(5)
_cell_measurement_reflns_used    21924
_cell_measurement_temperature    273.00(10)
_cell_measurement_theta_max      77.4390
_cell_measurement_theta_min      2.9540
_cell_volume                     6890.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      273.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_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    -83.00 -46.00   1.00    1.50    --  -51.89 -43.00 -99.00   37
  2  \w    -30.00  24.00   1.00    1.50    --  -51.89  43.00  51.00   54
  3  \w    -19.00   7.00   1.00    1.50    --   51.89 -43.00 -99.00   26
  4  \w     44.00 112.00   1.00    1.50    --   51.89  43.00  51.00   68
  5  \w   -143.00 -78.00   1.00    5.50    --  -87.58 -43.00 -99.00   65
  6  \w     28.00  54.00   1.00    5.50    --  102.12 -43.00 -99.00   26
  7  \w     92.00 154.00   1.00    5.50    --  102.12  43.00  51.00   62
  8  \w    -44.00 -11.00   1.00    1.50    --    6.00 122.00 178.16   33
  9  \w     -3.00  24.00   1.00    1.50    --  -51.89  19.00 -30.00   27
 10  \w     -4.00  21.00   1.00    1.50    --  -51.89  19.00-180.00   25
 11  \w   -154.00 -87.00   1.00    5.50    --  -87.58 -99.00  60.00   67
 12  \w     25.00  51.00   1.00    5.50    --  102.12 -38.00 -60.00   26
 13  \w    143.00 172.00   1.00    5.50    --  102.12 125.00 -60.00   29
 14  \w     44.00  77.00   1.00    5.50    --  102.12 -57.00-180.00   33
 15  \w     25.00  51.00   1.00    5.50    --  102.12 -38.00 120.00   26
 16  \w     37.00  66.00   1.00    5.50    --  102.12 -57.00 -60.00   29
 17  \w    104.00 175.00   1.00    5.50    --  102.12  38.00  90.00   71
 18  \w     25.00  51.00   1.00    5.50    --  102.12 -38.00 -30.00   26
 19  \w     87.00 134.00   1.00    5.50    --  102.12 125.00 -60.00   47
 20  \w     26.00  52.00   1.00    5.50    --  102.12 -38.00  90.00   26
 21  \w     42.00  93.00   1.00    5.50    --  107.25 -86.00-109.69   51
 22  \w     51.00  76.00   1.00    5.50    --  107.25 -65.00 -49.27   25
 23  \w     97.00 127.00   1.00    5.50    --  107.25-147.00 146.59   30
 24  \w     38.00  94.00   1.00    5.50    --  107.25-147.00 146.59   56
 25  \w    106.00 163.00   1.00    5.50    --  107.25   3.00 -23.04   57
 26  \w     45.00  86.00   1.00    5.50    --  107.25 -66.00  21.08   41
 27  \w     39.00  86.00   1.00    5.50    --  107.25   3.00 -23.04   47
 28  \w     44.00 130.00   1.00    5.50    --  107.25 -79.00 -66.96   86
 29  \w     68.00 141.00   1.00    5.50    --  107.25  19.00-135.88   73
 30  \w     59.00  90.00   1.00    5.50    --  107.25 -63.00 163.26   31
 31  \w    142.00 175.00   1.00    5.50    --  107.25 112.00 -93.21   33
 32  \w     99.00 126.00   1.00    5.50    --  107.25 -81.00 167.35   27
 33  \w     62.00  88.00   1.00    5.50    --  107.25-116.00-101.18   26
 34  \w     43.00  89.00   1.00    5.50    --  107.25 -81.00 167.35   46
 35  \w     40.00  76.00   1.00    5.50    --  107.25 -73.00  -8.76   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0341867000
_diffrn_orient_matrix_UB_12      -0.0263049000
_diffrn_orient_matrix_UB_13      -0.0774694000
_diffrn_orient_matrix_UB_21      -0.1118348000
_diffrn_orient_matrix_UB_22      0.0112049000
_diffrn_orient_matrix_UB_23      -0.0038977000
_diffrn_orient_matrix_UB_31      0.0082779000
_diffrn_orient_matrix_UB_32      0.0432744000
_diffrn_orient_matrix_UB_33      -0.0461043000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74695
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.445
_diffrn_reflns_theta_min         2.977
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         14655
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1234P)^2^+8.7724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11541
_reflns_number_total             14655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-185n-dry-273k_r_abs
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_database_code               7248792
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H14 N4 O6 S1 Ni1'
_chemical_oxdiff_usercomment     'light blue/green block'
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N37-C38A \\sim N37-C38B
 with sigma of 0.02
 N37-C41A \\sim N37-C41B
 with sigma of 0.02
 N39-C38A \\sim N39-C38B
 with sigma of 0.02
 N39-C40A \\sim N39-C40B
 with sigma of 0.02
 C41A-C40A \\sim C41B-C40B
 with sigma of 0.02
 N37-C40A \\sim N37-C40B
 with sigma of 0.04
 N39-C41A \\sim N39-C41B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C5) = Uanis(C4)
Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C6) = Uanis(C12) = Uanis(C11) =
Uanis(C10)
4. Others
 Fixed Sof: C38A(0.55) H38A(0.55) C41A(0.55) H41A(0.55) C40A(0.55) H40A(0.55)
 C40B(0.45) H40B(0.45) C41B(0.45) H41B(0.45) C38B(0.45) H38B(0.45)
5.a Rotating group:
 O77(H77A,H77B)
5.b Aromatic/amide H refined with riding coordinates:
 C65(H65), C67(H67), C69(H69), C2(H2), C14(H14), C57(H57), C33(H33),
 C38A(H38A), C17(H17), C16(H16), C35(H35), C59(H59), C23(H23), C5(H5), C20(H20),
  C36(H36), C51(H51), C54(H54), C47(H47), C30(H30), C60(H60), C52(H52), C4(H4),
 C27(H27), C44(H44), C21(H21), C22(H22), C53(H53), C29(H29), C28(H28), C45(H45),
  C46(H46), C41A(H41A), C40A(H40A), C40B(H40B), C41B(H41B), C38B(H38B),
 C11(H11), C8(H8), C10(H10), C9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              81753
_shelx_fab_checksum              76729
_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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.751