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_7248793
_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(H2 O), 6(C3 H7 N O)'
_chemical_formula_sum            'C134 H146 N26 Ni3 O34 S2'
_chemical_formula_weight         2905.01
_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                 104.0130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.63110(10)
_cell_length_b                   30.64140(10)
_cell_length_c                   16.96660(10)
_cell_measurement_reflns_used    40685
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      78.6090
_cell_measurement_theta_min      3.0300
_cell_volume                     6875.65(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.984
_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    -54.00 -13.00   1.00    2.00    --  -87.71  57.00  30.00   41
  2  \w     -3.00  23.00   1.00    1.00    --  -54.15  19.00 -30.00   26
  3  \w    -51.00 -13.00   1.00    2.00    --  -87.71  57.00 -60.00   38
  4  \w    -24.00  20.00   1.00    1.00    --  -54.15  35.00-116.00   44
  5  \w    -30.00  -5.00   1.00    1.00    --   14.00 112.00  -4.51   25
  6  \w    -54.00 -29.00   1.00    1.00    --   18.00 154.00-149.09   25
  7  \w     95.00 127.00   1.00    2.00    --  107.25 139.00  48.60   32
  8  \w    145.00 173.00   1.00    2.00    --  107.25 139.00  48.60   28
  9  \w     37.00 101.00   1.00    1.00    --   52.65  35.00-116.00   64
 10  \w     77.00 104.00   1.00    2.00    --  106.00  20.00-135.90   27
 11  \w     86.00 122.00   1.00    2.00    --  101.96  35.00-116.00   36
 12  \w    134.00 176.00   1.00    2.00    --  101.96  35.00-116.00   42
 13  \w    150.00 175.00   1.00    2.00    --  106.00  20.00-135.90   25
 14  \w    123.00 172.00   1.00    2.00    --  107.25  32.00 -22.88   49
 15  \w     48.00  76.00   1.00    2.00    --  107.25 -78.00-111.66   28
 16  \w     36.00  70.00   1.00    2.00    --  107.25 -66.00-142.47   34
 17  \w     34.00  79.00   1.00    2.00    --  101.96 -57.00 -90.00   45
 18  \w    101.00 132.00   1.00    2.00    --  107.25 -78.00-111.66   31
 19  \w     39.00  72.00   1.00    2.00    --  107.25 -57.00-122.12   33
 20  \w     33.00  61.00   1.00    2.00    --  107.25 -52.00 -71.91   28
 21  \w     37.00  71.00   1.00    2.00    --  107.25 -55.00 -49.88   34
 22  \w     59.00  85.00   1.00    2.00    --  107.25 -67.00 -19.91   26
 23  \w     30.00  55.00   1.00    2.00    --  107.25 -43.00  63.79   25
 24  \w     38.00  68.00   1.00    2.00    --  107.25 -51.00  99.72   30
 25  \w     31.00  56.00   1.00    2.00    --  107.25 -42.00 138.20   25
 26  \w     25.00  50.00   1.00    2.00    --  101.96 -38.00 120.00   25
 27  \w     25.00  50.00   1.00    2.00    --  101.96 -38.00  90.00   25
 28  \w     27.00  52.00   1.00    2.00    --  101.96 -38.00-150.00   25
 29  \w     30.00  55.00   1.00    2.00    --  107.25 -41.00 -31.72   25
 30  \w    -20.00  45.00   1.00    1.00    --   52.65 -35.00  86.00   65
 31  \w     27.00  52.00   1.00    2.00    --  101.96 -38.00 150.00   25
 32  \w     54.00 110.00   1.00    2.00    --  107.25 -73.00 108.74   56
 33  \w     38.00 104.00   1.00    2.00    --  101.96 -99.00 120.00   66
 34  \w     48.00  92.00   1.00    2.00    --  107.25-165.00 151.04   44
 35  \w     96.00 131.00   1.00    2.00    --  107.25-165.00 151.04   35
 36  \w     45.00 119.00   1.00    2.00    --  107.25-158.00  91.56   74
 37  \w     38.00  65.00   1.00    2.00    --  107.25-103.00-138.89   27
 38  \w     69.00  95.00   1.00    2.00    --  107.25-103.00-138.89   26
 39  \w    -63.00 -38.00   1.00    1.00    --  -54.15 -35.00  86.00   25
 40  \w   -131.00 -84.00   1.00    1.00    --  -54.15 -35.00  86.00   47
 41  \w   -143.00-118.00   1.00    2.00    --  -87.71 -35.00  86.00   25
;
_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      -0.0265367000
_diffrn_orient_matrix_UB_12      0.0221656000
_diffrn_orient_matrix_UB_13      0.0736343000
_diffrn_orient_matrix_UB_21      0.1100802000
_diffrn_orient_matrix_UB_22      -0.0057725000
_diffrn_orient_matrix_UB_23      0.0492374000
_diffrn_orient_matrix_UB_31      0.0273719000
_diffrn_orient_matrix_UB_32      0.0447637000
_diffrn_orient_matrix_UB_33      -0.0301428000
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75492
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.076
_diffrn_reflns_theta_min         2.884
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_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    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0694P)^2^+8.9673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13557
_reflns_number_total             14648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-185h_r_abs_2
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_database_code               7248793
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H20 N6 O4 S1 Ni1'
_chemical_oxdiff_usercomment     'light green block'
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O98A(0.8) H98A(0.8) H98B(0.8) O98B(0.2) H98C(0.2) H98D(0.2)
3.a Free rotating group:
 O94(H94A,H94B), O95(H95A,H95B), O96(H96A,H96B), O97(H97A,H97B), O83(H83A,
 H83B), O98A(H98A,H98B), O98B(H98C,H98D)
3.b Rotating group:
 O77(H77A,H77B)
3.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C2(H2), C65(H65), C69(H69), C67(H67), C14(H14), C36(H36), C57(H57),
 C35(H35), C17(H17), C41(H41), C5(H5), C54(H54), C33(H33), C4(H4), C27(H27),
 C30(H30), C16(H16), C53(H53), C23(H23), C8(H8), C28(H28), C11(H11), C40(H40),
 C29(H29), C20(H20), C51(H51), C52(H52), C44(H44), C21(H21), C22(H22), C47(H47),
  C9(H9), C10(H10), C87(H87), C59(H59), C45(H45), C60(H60), C46(H46), C81(H81),
 C92(H92)
3.d Idealised Me refined as rotating group:
 C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C78(H78A,H78B,H78C), C89(H89A,H89B,
 H89C), C79(H79A,H79B,H79C), C90(H90A,H90B,H90C)
;
_shelx_res_checksum              40234
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.899