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_7248791
_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         'C72 H44 Cu8 N8 O32 S4'
_chemical_formula_sum            'C72 H44 Cu8 N8 O32 S4'
_chemical_formula_weight         2169.71
_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             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                88.5480(10)
_cell_angle_beta                 89.922(2)
_cell_angle_gamma                84.669(2)
_cell_formula_units_Z            1
_cell_length_a                   10.1534(2)
_cell_length_b                   10.8388(2)
_cell_length_c                   17.2424(2)
_cell_measurement_reflns_used    16747
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      77.2570
_cell_measurement_theta_min      4.7650
_cell_volume                     1888.72(6)
_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_temperature      120.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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    -16.00  24.00   0.50    2.00    --  -51.89  48.00  23.00   80
  2  \w   -127.00 -46.00   0.50    2.00    --  -51.89 -48.00-124.00  162
  3  \w     58.00  83.00   0.50    2.00    --   51.89  48.00  23.00   50
  4  \w    -23.00  40.00   0.50    2.00    --   51.89 -48.00-124.00  126
  5  \w   -159.00-133.00   0.50    7.00    --  -87.58 -48.00-124.00   52
  6  \w    -40.00 -13.00   0.50    7.00    --  -87.58  48.00  23.00   54
  7  \w     31.00  63.00   0.50    7.00    --  102.12 -48.00-124.00   64
  8  \w     88.00 176.00   0.50    7.00    --  102.12  48.00  23.00  176
  9  \w    -45.00 -13.00   0.50    2.00    --    6.00 125.00 -18.47   64
 10  \w    -28.00  -3.00   0.50    2.00    --   14.00 109.00-128.89   50
 11  \w     -4.00  25.00   0.50    2.00    --  -51.89  19.00-180.00   58
 12  \w    -52.00 -14.00   0.50    7.00    --  -87.58  57.00-180.00   76
 13  \w   -116.00 -89.00   0.50    7.00    --  -87.58 -48.00-124.00   54
 14  \w    -54.00 -15.00   0.50    7.00    --  -87.58  57.00 120.00   78
 15  \w    -51.00 -13.00   0.50    7.00    --  -87.58  57.00 -30.00   76
 16  \w     59.00 109.00   0.50    7.00    --  102.12-125.00-150.00  100
 17  \w     61.00 105.00   0.50    7.00    --  102.12 -99.00 -60.00   88
 18  \w     89.00 170.00   0.50    7.00    --  102.12  38.00 -30.00  162
 19  \w     25.00  50.00   0.50    7.00    --  102.12 -38.00 -30.00   50
 20  \w     84.00 111.00   0.50    7.00    --  102.12-125.00 -60.00   54
 21  \w    129.00 157.00   0.50    7.00    --  102.12 125.00 150.00   56
 22  \w     25.00  52.00   0.50    7.00    --  102.12 -38.00  30.00   54
 23  \w     26.00  52.00   0.50    7.00    --  102.12 -38.00 -60.00   52
 24  \w     25.00  51.00   0.50    7.00    --  102.12 -38.00  90.00   52
 25  \w     79.00 111.00   0.50    7.00    --  102.12-125.00 -30.00   64
 26  \w     78.00 106.00   0.50    7.00    --  102.12 -99.00 150.00   56
 27  \w     26.00  51.00   0.50    7.00    --  102.12 -38.00  60.00   50
 28  \w     75.00 111.00   0.50    7.00    --  102.12-125.00  90.00   72
 29  \w     80.00 106.00   0.50    7.00    --  102.12 -99.00-120.00   52
 30  \w     68.00 106.00   0.50    7.00    --  102.12 -99.00  90.00   76
 31  \w     28.00  56.00   0.50    7.00    --  102.12 -57.00-150.00   56
 32  \w    132.00 176.00   0.50    7.00    --  102.12  38.00  60.00   88
 33  \w     30.00  55.00   0.50    7.00    --  102.12 -57.00-180.00   50
 34  \w     80.00 106.00   0.50    7.00    --  102.12 -99.00  60.00   52
 35  \w     70.00 106.00   0.50    7.00    --  102.12 -99.00   0.00   72
 36  \w     79.00 105.00   0.50    7.00    --  102.12 -99.00-180.00   52
 37  \w    103.00 129.00   0.50    7.00    --  102.12  38.00  60.00   52
 38  \w    122.00 148.00   0.50    7.00    --  107.25 123.00  12.76   52
 39  \w    120.00 160.00   0.50    7.00    --  107.25   2.00-130.87   80
 40  \w    115.00 155.00   0.50    7.00    --  107.25 141.00  96.45   80
 41  \w     69.00 123.00   0.50    7.00    --  107.25 -85.00 179.59  108
 42  \w     69.00  95.00   0.50    7.00    --  107.25 141.00  96.45   52
 43  \w     41.00  89.00   0.50    7.00    --  107.25 -70.00-124.67   96
 44  \w     38.00 102.00   0.50    7.00    --  107.25-122.00 178.47  128
 45  \w     42.00  89.00   0.50    7.00    --  107.25 -81.00  -5.66   94
 46  \w     30.00  55.00   0.50    7.00    --  107.25 -41.00  13.18   50
 47  \w     41.00 111.00   0.50    7.00    --  107.25 -83.00  75.05  140
 48  \w    119.00 176.00   0.50    7.00    --  107.25  23.00 161.46  114
 49  \w     85.00 110.00   0.50    7.00    --  107.25  23.00 161.46   50
 50  \w     49.00  74.00   0.50    7.00    --  107.25 -73.00  41.21   50
 51  \w     87.00 115.00   0.50    7.00    --  107.25 -85.00-138.74   56
 52  \w     55.00  82.00   0.50    7.00    --  107.25 -85.00-138.74   54
 53  \w     83.00 109.00   0.50    7.00    --  107.25 -87.00 115.66   52
 54  \w     44.00  90.00   0.50    7.00    --  107.25 -69.00 114.35   92
 55  \w    134.00 174.00   0.50    7.00    --  107.25  17.00-106.43   80
 56  \w     70.00 102.00   0.50    7.00    --  107.25  17.00-106.43   64
 57  \w     33.00  71.00   0.50    7.00    --  107.25 -54.00 148.35   76
 58  \w     94.00 137.00   0.50    7.00    --  107.25 -88.00 -64.06   86
 59  \w     41.00  91.00   0.50    7.00    --  107.25 -88.00 -64.06  100
 60  \w    109.00 135.00   0.50    7.00    --  107.25  59.00 -55.11   52
 61  \w     43.00  71.00   0.50    7.00    --  107.25 -86.00-145.34   56
 62  \w     71.00 143.00   0.50    7.00    --  107.25  16.00 -26.51  144
 63  \w     65.00 106.00   0.50    7.00    --  107.25  18.00 154.65   82
 64  \w     39.00  78.00   0.50    7.00    --  107.25 -71.00  92.29   78
;
_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      -0.1010778000
_diffrn_orient_matrix_UB_12      0.0995468000
_diffrn_orient_matrix_UB_13      0.0334056000
_diffrn_orient_matrix_UB_21      0.0721633000
_diffrn_orient_matrix_UB_22      0.1020952000
_diffrn_orient_matrix_UB_23      -0.0411091000
_diffrn_orient_matrix_UB_31      -0.0883046000
_diffrn_orient_matrix_UB_32      -0.0076181000
_diffrn_orient_matrix_UB_33      -0.0719872000
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.527
_diffrn_reflns_theta_min         2.563
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.302
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.974
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.043
_exptl_crystal_size_mid          0.024
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8038
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0551P)^2^+5.5688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6949
_reflns_number_total             8038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-148l-h2o_r_abs_2
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_database_code               7248791
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H14 N6 Cu1 O4 S1'
_chemical_oxdiff_usercomment     'Green small block'
_shelx_estimated_absorpt_t_max   0.923
_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) groups
2. Restrained distances
 S52-O53A \\sim S52-O54B
 with sigma of 0.02
 S52-O55A \\sim S52-O53B
 with sigma of 0.02
 S52-O54A \\sim S52-O55B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O54B) \\sim Ueq, Uanis(O53B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O54B) = Uanis(O54A) = Uanis(O53B) = Uanis(O55A) = Uanis(O53A) =
Uanis(O55B)
4. Others
 Fixed Sof: O53A(0.9) O55A(0.9) O54A(0.9) O54B(0.1) O55B(0.1) O53B(0.1)
5.a Ternary CH refined with riding coordinates:
 O13(H13), O42(H42)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C47(H47), C51(H51), C49(H49), C20(H20), C22(H22), C34(H34), C5(H5),
 C2(H2), C32(H32), C37(H37), C40(H40), C31(H31), C3(H3), C39(H39), C38(H38),
 C8(H8), C11(H11), C9(H9), C10(H10)
;
_shelx_res_checksum              12272
_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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.732