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_7248790
_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         'C48 H32 N9 Ni O4, C28 H22 N5 Ni O6, 0.5(H2 O)'
_chemical_formula_sum            'C76 H55 N14 Ni2 O10.5'
_chemical_formula_weight         1449.76
_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   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                61.328(11)
_cell_angle_beta                 71.172(9)
_cell_angle_gamma                75.382(10)
_cell_formula_units_Z            1
_cell_length_a                   11.2569(11)
_cell_length_b                   13.4025(17)
_cell_length_c                   13.5086(13)
_cell_measurement_reflns_used    5691
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      78.4760
_cell_measurement_theta_min      3.7840
_cell_volume                     1680.8(4)
_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      120.01(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 0.996
_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    -74.00  16.00   2.00    2.00    --  -51.06  87.00  46.00   45
  2  \w     19.00  47.00   2.00    2.00    --   51.81 -87.00 -70.00   14
  3  \w   -105.00 -75.00   2.00    9.00    --  -87.69  87.00  46.00   15
  4  \w   -154.00 -82.00   2.00    9.00    --  -87.69 -87.00 -70.00   36
  5  \w    140.00 166.00   2.00    9.00    --  101.97  87.00  46.00   13
  6  \w     83.00 131.00   2.00    9.00    --  101.97 -87.00 -70.00   24
  7  \w    -20.00  14.00   2.00    2.00    --   18.00 102.00  99.85   17
  8  \w     12.00  42.00   2.00    2.00    --   42.00  87.00-168.46   15
  9  \w     -2.00  24.00   2.00    2.00    --  -51.06  19.00 -90.00   13
 10  \w     37.00 125.00   2.00    2.00    --   58.00  75.00 -44.93   44
 11  \w   -136.00 -50.00   2.00    2.00    --  -66.00 -71.00 131.43   43
 12  \w   -153.00 -87.00   2.00    9.00    --  -87.69 -99.00  60.00   33
 13  \w     43.00 105.00   2.00    9.00    --  101.97 -99.00  90.00   31
 14  \w     25.00  51.00   2.00    9.00    --  101.97 -38.00-180.00   13
 15  \w     63.00  89.00   2.00    9.00    --  101.97-125.00  60.00   13
 16  \w     28.00  78.00   2.00    9.00    --  101.97 -57.00 -60.00   25
 17  \w     35.00  61.00   2.00    9.00    --  101.97 -57.00   0.00   13
 18  \w     30.00  76.00   2.00    9.00    --  101.97 -57.00-180.00   23
 19  \w     25.00  51.00   2.00    9.00    --  101.97 -38.00-150.00   13
 20  \w     68.00  94.00   2.00    9.00    --  101.97-125.00 -90.00   13
 21  \w     90.00 176.00   2.00    9.00    --  107.25  57.00 101.10   43
 22  \w    144.00 174.00   2.00    9.00    --  107.25  80.00 -13.95   15
 23  \w    129.00 175.00   2.00    9.00    --  107.25  60.00-167.89   23
 24  \w     86.00 118.00   2.00    9.00    --  107.25  80.00 -13.95   16
 25  \w    110.00 174.00   2.00    9.00    --  107.25  71.00  56.75   32
 26  \w    105.00 131.00   2.00    9.00    --  107.25 -83.00-117.80   13
 27  \w     77.00 105.00   2.00    9.00    --  107.25-100.00-127.38   14
 28  \w    137.00 175.00   2.00    9.00    --  107.25   7.00  59.06   19
 29  \w     42.00  82.00   2.00    9.00    --  107.25   7.00  59.06   20
 30  \w     41.00  77.00   2.00    9.00    --  107.25 -83.00-117.80   18
 31  \w     74.00 120.00   2.00    9.00    --  107.25-136.00-107.64   23
 32  \w     42.00  88.00   2.00    9.00    --  107.25 -72.00 -90.28   23
 33  \w     68.00 108.00   2.00    9.00    --  107.25-113.00  35.90   20
 34  \w     93.00 123.00   2.00    9.00    --  107.25  64.00 151.05   15
 35  \w     40.00 106.00   2.00    9.00    --  107.25 -99.00 -44.94   33
 36  \w     48.00  74.00   2.00    9.00    --  107.25-115.00   7.27   13
 37  \w    147.00 173.00   2.00    9.00    --  107.25  49.00 -96.87   13
 38  \w     67.00  95.00   2.00    9.00    --  107.25 -68.00  42.37   14
 39  \w     46.00 106.00   2.00    9.00    --  107.25-100.00 155.07   30
 40  \w    100.00 128.00   2.00    9.00    --  107.25  49.00 -96.87   14
 41  \w     99.00 173.00   2.00    9.00    --  107.25 106.00 -53.07   37
 42  \w     87.00 173.00   2.00    9.00    --  107.25  71.00 166.11   43
 43  \w     80.00 108.00   2.00    9.00    --  107.25-117.00 -65.39   14
 44  \w    148.00 176.00   2.00    9.00    --  107.25 107.00 175.02   14
 45  \w     54.00 106.00   2.00    9.00    --  107.25-104.00 139.77   26
 46  \w    144.00 170.00   2.00    9.00    --  107.25  64.00 151.05   13
 47  \w     55.00  81.00   2.00    9.00    --  107.25 -75.00 136.45   13
 48  \w     92.00 118.00   2.00    9.00    --  107.25 -84.00  -3.44   13
 49  \w     91.00 145.00   2.00    9.00    --  107.25  28.00 157.65   27
;
_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      0.0276022000
_diffrn_orient_matrix_UB_12      -0.1156439000
_diffrn_orient_matrix_UB_13      -0.0063452000
_diffrn_orient_matrix_UB_21      -0.1250145000
_diffrn_orient_matrix_UB_22      0.0249040000
_diffrn_orient_matrix_UB_23      -0.0358146000
_diffrn_orient_matrix_UB_31      0.0693442000
_diffrn_orient_matrix_UB_32      0.0583949000
_diffrn_orient_matrix_UB_33      -0.1287714000
_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  0.0842
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.994
_diffrn_reflns_theta_min         3.785
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.906
_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    1.432
_exptl_crystal_description       plank
_exptl_crystal_F_000             749
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0531P)^2^+2.0795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4828
_reflns_number_total             6775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-177e_r_abs_2
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_original_formula_sum        'C76 H55 N14 Ni2 O10.50'
_cod_database_code               7248790
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H20 N6 O6 Ni1'
_chemical_oxdiff_usercomment     'green rod'
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: N7(0.5) H7A(0.5) H7B(0.5) N38(0.5) H38A(0.5) H38B(0.5) O52(0.25)
 H52A(0.25) H52B(0.25)
3.a Free rotating group:
 O52(H52A,H52B)
3.b Rotating group:
 O51(H51A,H51B), N7(H7A,H7B), N38(H38A,H38B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C21(H21), C12(H12), C5(H5), C11(H11), C15(H15), C18(H18), C49(H49),
 C42(H42), C46(H46), C36(H36), C17(H17), C40(H40), C24(H24), C43(H43), C27(H27),
  C16(H16), C47(H47), C23(H23), C30(H30), C48(H48), C28(H28), C29(H29)
;
_shelx_res_checksum              77602
_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 1.540
_oxdiff_exptl_absorpt_empirical_full_min 0.657