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_7248789
_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         'C56 H38 N10 Ni2 O8, 5(H2 O)'
_chemical_formula_sum            'C56 H48 N10 Ni2 O13'
_chemical_formula_weight         1186.46
_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             2023-11-20
_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                 96.771(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1841(2)
_cell_length_b                   22.1378(4)
_cell_length_c                   12.2623(2)
_cell_measurement_reflns_used    8745
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.5680
_cell_measurement_theta_min      4.1240
_cell_volume                     2745.30(9)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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 -51.00   1.00   14.00    --  -48.63 -44.00 174.00   32
  2  \w    -23.00  29.00   1.00   14.00    --  -48.63  44.00 -35.00   52
  3  \w     51.00  96.00   1.00   14.00    --   49.50  44.00 -35.00   45
  4  \w    -28.00  53.00   1.00   14.00    --   49.50 -44.00 174.00   81
  5  \w   -125.00 -99.00   1.00   36.00    --  -88.21 -44.00 174.00   26
  6  \w    -45.00 -17.00   1.00   36.00    --  -88.21  44.00 -35.00   28
  7  \w    125.00 175.00   1.00   36.00    --  104.82  44.00 -35.00   50
  8  \w     27.00  52.00   1.00   36.00    --  104.82 -44.00 174.00   25
  9  \w   -120.00 -74.00   1.00   14.00    --  -48.63-125.00 -30.00   46
 10  \w    -38.00 -11.00   1.00   36.00    --  -88.21  45.00 -90.00   27
 11  \w    -44.00 -11.00   1.00   36.00    --  -88.21  45.00  60.00   33
 12  \w   -127.00 -87.00   1.00   36.00    --  -88.21 -95.00 -60.00   40
 13  \w    -47.00 -22.00   1.00   36.00    --  -88.21  45.00 -60.00   25
 14  \w    -44.00 -15.00   1.00   36.00    --  -88.21  45.00  90.00   29
 15  \w    -41.00 -10.00   1.00   36.00    --  -88.21  45.00  30.00   31
 16  \w    -46.00 -13.00   1.00   36.00    --  -88.21  45.00   0.00   33
 17  \w    -47.00 -11.00   1.00   36.00    --  -88.21  45.00-120.00   36
 18  \w    -62.00 -15.00   1.00   36.00    --  -88.21  61.00 120.00   47
 19  \w    127.00 175.00   1.00   36.00    --  104.82  30.00   0.00   48
 20  \w     44.00  70.00   1.00   36.00    --  104.82 -95.00 150.00   26
 21  \w    138.00 171.00   1.00   36.00    --  104.82  45.00-150.00   33
 22  \w     49.00  74.00   1.00   36.00    --  104.82 -61.00-150.00   25
 23  \w     39.00  95.00   1.00   36.00    --  104.82 -95.00  30.00   56
 24  \w     48.00  77.00   1.00   36.00    --  104.82 -77.00-150.00   29
 25  \w     95.00 121.00   1.00   36.00    --  104.82  45.00-150.00   26
 26  \w     27.00  53.00   1.00   36.00    --  104.82 -45.00 120.00   26
 27  \w     57.00  94.00   1.00   36.00    --  104.82 -95.00  90.00   37
 28  \w     32.00  74.00   1.00   36.00    --  104.82 -61.00  30.00   42
 29  \w    132.00 158.00   1.00   36.00    --  104.82 125.00  30.00   26
 30  \w     38.00  64.00   1.00   36.00    --  104.82 -95.00 -30.00   26
 31  \w     67.00 102.00   1.00   36.00    --  104.82 -95.00 -30.00   35
 32  \w     54.00 131.00   1.00   36.00    --  104.82  15.00 -30.00   77
 33  \w    140.00 166.00   1.00   36.00    --  104.82  30.00  90.00   26
 34  \w     80.00 105.00   1.00   36.00    --  104.82 -95.00 150.00   25
 35  \w    137.00 162.00   1.00   36.00    --  104.82  30.00-120.00   25
 36  \w     95.00 167.00   1.00   36.00    --  104.82  15.00  60.00   72
 37  \w     41.00  67.00   1.00   36.00    --  104.82 -61.00  60.00   26
 38  \w     59.00  85.00   1.00   36.00    --  104.82  15.00 150.00   26
 39  \w    103.00 133.00   1.00   36.00    --  104.82  30.00-120.00   30
 40  \w     41.00  67.00   1.00   36.00    --  104.82  15.00  60.00   26
 41  \w    100.00 178.00   1.00   36.00    --  104.82  15.00 150.00   78
 42  \w     95.00 120.00   1.00   36.00    --  104.82  45.00  90.00   25
 43  \w     28.00  54.00   1.00   36.00    --  104.82 -45.00  90.00   26
 44  \w     88.00 114.00   1.00   36.00    --  104.82 125.00  30.00   26
 45  \w     27.00  52.00   1.00   36.00    --  104.82 -45.00 -30.00   25
 46  \w     27.00  52.00   1.00   36.00    --  104.82 -45.00   0.00   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      -0.0082104000
_diffrn_orient_matrix_UB_12      0.0140450000
_diffrn_orient_matrix_UB_13      0.1220491000
_diffrn_orient_matrix_UB_21      0.1294561000
_diffrn_orient_matrix_UB_22      0.0364372000
_diffrn_orient_matrix_UB_23      0.0049829000
_diffrn_orient_matrix_UB_31      -0.0798503000
_diffrn_orient_matrix_UB_32      0.0576151000
_diffrn_orient_matrix_UB_33      -0.0328849000
_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  0.0848
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30247
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.555
_diffrn_reflns_theta_min         3.994
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.946
_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    1.435
_exptl_crystal_description       plank
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0494P)^2^+4.2789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4147
_reflns_number_total             5747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-165-b_1r_abs
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_database_code               7248789
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H20 N6 Ni1 O4'
_chemical_oxdiff_usercomment     'no. 60'
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.843
_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
 N22-H22B = N22-H22A
 0.99 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O40A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O38B(0.3) H38A(0.3) H38B(0.3) O38A(0.7) H38C(0.7) H38D(0.7)
 O40A(0.5) H40A(0.5) H40B(0.5)
5.a Free rotating group:
 O39(H39A,H39B), O38B(H38A,H38B), O38A(H38C,H38D), O40A(H40A,H40B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C27(H27), C19(H19), C21(H21), C2(H2), C8(H8), C36(H36), C11(H11),
 C4(H4), C33(H33), C5(H5), C30(H30), C9(H9), C10(H10), C29(H29), C35(H35),
 C34(H34)
;
_shelx_res_checksum              4970
_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 2.054
_oxdiff_exptl_absorpt_empirical_full_min 0.561