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_7248794
_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, 4[C3H7NO], 14[H2O]'
_chemical_formula_sum            'C128 H136 N24 Ni3 O34 S2'
_chemical_formula_weight         2794.85
_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                 104.0980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.61780(10)
_cell_length_b                   29.7718(2)
_cell_length_c                   17.1157(2)
_cell_measurement_reflns_used    31802
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      78.6090
_cell_measurement_theta_min      2.9890
_cell_volume                     6730.15(11)
_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      N~2~
_diffrn_ambient_temperature      120.00(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 0.998
_diffrn_measured_fraction_theta_max 0.985
_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    -29.00  -4.00   1.00    0.20    --   14.00 110.00-150.99   25
  2  \w    -44.00 -19.00   1.00    1.00    --  -87.58  57.00 -60.00   25
  3  \w    -37.00 -11.00   1.00    1.00    --  -87.58  46.00  92.00   26
  4  \w    -36.00  19.00   1.00    0.20    --  -51.89  46.00  92.00   55
  5  \w     -2.00  23.00   1.00    0.20    --   34.00  98.00 179.40   25
  6  \w     91.00 174.00   1.00    1.00    --  107.25  94.00  85.31   83
  7  \w     40.00 123.00   1.00    0.20    --   51.89  46.00  92.00   83
  8  \w    115.00 154.00   1.00    1.00    --  102.12  46.00  92.00   39
  9  \w    129.00 155.00   1.00    1.00    --  107.25  46.00  75.75   26
 10  \w     43.00 114.00   1.00    1.00    --  107.25   8.00-102.71   71
 11  \w     25.00  50.00   1.00    1.00    --  102.12 -38.00-180.00   25
 12  \w     41.00  73.00   1.00    1.00    --  107.25 -76.00-146.10   32
 13  \w     47.00  73.00   1.00    1.00    --  107.25 -73.00-120.92   26
 14  \w     76.00 117.00   1.00    1.00    --  107.25 -73.00-120.92   41
 15  \w     42.00  71.00   1.00    1.00    --  102.12 -57.00 -90.00   29
 16  \w     51.00  86.00   1.00    1.00    --  107.25 -61.00  14.26   35
 17  \w     35.00  88.00   1.00    1.00    --  107.25 -62.00  57.53   53
 18  \w     28.00  64.00   1.00    1.00    --  102.12 -57.00  90.00   36
 19  \w     35.00  61.00   1.00    1.00    --  102.12 -57.00 150.00   26
 20  \w     34.00  84.00   1.00    1.00    --  107.25 -60.00 119.62   50
 21  \w     29.00  55.00   1.00    1.00    --  102.12 -46.00 -57.00   26
 22  \w     29.00  70.00   1.00    1.00    --  102.12 -57.00-120.00   41
 23  \w     33.00  63.00   1.00    1.00    --  107.25 -56.00-155.83   30
 24  \w     25.00  50.00   1.00    1.00    --  102.12 -38.00   0.00   25
 25  \w     25.00  50.00   1.00    1.00    --  102.12 -38.00 -30.00   25
 26  \w    -23.00  58.00   1.00    0.20    --   51.89 -46.00 -57.00   81
 27  \w     25.00  50.00   1.00    1.00    --  102.12 -38.00  90.00   25
 28  \w    111.00 136.00   1.00    1.00    --  107.25 -84.00 -24.62   25
 29  \w     80.00 129.00   1.00    1.00    --  107.25 -88.00  11.98   49
 30  \w     41.00  76.00   1.00    1.00    --  107.25 -88.00  11.98   35
 31  \w     55.00  97.00   1.00    1.00    --  107.25 -84.00 -24.62   42
 32  \w     48.00 104.00   1.00    1.00    --  107.25-122.00-128.96   56
 33  \w   -112.00 -76.00   1.00    1.00    --  -87.58 -46.00 -57.00   36
 34  \w   -162.00-119.00   1.00    1.00    --  -87.58 -46.00 -57.00   43
 35  \w   -154.00 -87.00   1.00    1.00    --  -87.58 -99.00  60.00   67
 36  \w    -83.00 -37.00   1.00    0.20    --  -51.89 -46.00 -57.00   46
;
_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      -0.0771476000
_diffrn_orient_matrix_UB_12      0.0278587000
_diffrn_orient_matrix_UB_13      -0.0619654000
_diffrn_orient_matrix_UB_21      0.0808148000
_diffrn_orient_matrix_UB_22      0.0088437000
_diffrn_orient_matrix_UB_23      -0.0473955000
_diffrn_orient_matrix_UB_31      -0.0336525000
_diffrn_orient_matrix_UB_32      -0.0426801000
_diffrn_orient_matrix_UB_33      -0.0502710000
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73390
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.073
_diffrn_reflns_theta_min         2.969
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.737
_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    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.723
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         14350
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1010P)^2^+17.9068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2222
_refine_ls_wR_factor_ref         0.2267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12816
_reflns_number_total             14350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-185n-dry_r_abs
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_database_code               7248794
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H14 N4 O6 S1 Ni1'
_chemical_oxdiff_usercomment     'pale/light green cut block'
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.777
_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(N39) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C41B) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C40B) \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.1
Uanis(C38A) \\sim Ueq, Uanis(C38B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C53) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48) =
Uanis(C43) = Uanis(C55) = Uanis(C54) = Uanis(C52) = Uanis(C51) = Uanis(C50)
Uanis(N39) = Uanis(N37) = Uanis(N56) = Uanis(N58)
Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C7) = Uanis(C8) = Uanis(C9)
4. Others
 Fixed Sof: C38A(0.65) H38A(0.65) C41A(0.65) H41A(0.65) C40A(0.65) H40A(0.65)
 C41B(0.35) H41B(0.35) C40B(0.35) H40B(0.35) C38B(0.35) H38B(0.35)
5.a Rotating group:
 O77(H77A,H77B)
5.b Aromatic/amide H refined with riding coordinates:
 C65(H65), C14(H14), C67(H67), C57(H57), C2(H2), C17(H17), C69(H69), C33(H33),
 C27(H27), C20(H20), C16(H16), C5(H5), C59(H59), C29(H29), C47(H47), C23(H23),
 C28(H28), C4(H4), C30(H30), C21(H21), C35(H35), C36(H36), C22(H22), C60(H60),
 C8(H8), C51(H51), C11(H11), C54(H54), C44(H44), C46(H46), C52(H52), C45(H45),
 C9(H9), C53(H53), C10(H10), C38A(H38A), C41A(H41A), C40A(H40A), C41B(H41B),
 C40B(H40B), C38B(H38B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              71006
_shelx_fab_checksum              50662
_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 1.138
_oxdiff_exptl_absorpt_empirical_full_min 0.898