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_7248788
_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         '2(N O3), C20 H16 N4'
_chemical_formula_sum            'C20 H16 N6 O6'
_chemical_formula_weight         436.39
_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   geom
_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                 99.6960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.17230(10)
_cell_length_b                   10.30090(10)
_cell_length_c                   13.34380(10)
_cell_measurement_reflns_used    6750
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      77.3460
_cell_measurement_theta_min      5.4440
_cell_volume                     971.773(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.982
_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     41.00 118.00   0.50    1.00    --   52.72  65.00 130.00  154
  2  \w    -12.00  65.00   0.50    1.00    --   53.07 -65.00  -5.00  154
  3  \w     36.00 113.00   0.50    6.00    --  101.90 -65.00  -5.00  154
  4  \w     91.00 168.00   0.50    6.00    --  101.90  65.00 130.00  154
  5  \w    -46.00 -15.00   0.50    1.00    --    2.00 129.00 169.02   62
  6  \w    -13.00  31.00   0.50    1.00    --   14.00  95.00 136.96   88
  7  \w     12.00  41.00   0.50    1.00    --   38.00  92.00  13.96   58
  8  \w    -13.00  64.00   0.50    1.00    --   52.72 -65.00  -5.00  154
  9  \w     85.00 163.00   0.50    6.00    --  101.90  77.00  90.00  156
 10  \w     43.00 106.00   0.50    6.00    --  101.90 -99.00-150.00  126
 11  \w     43.00 106.00   0.50    6.00    --  101.90 -99.00   0.00  126
 12  \w     52.00 131.00   0.50    6.00    --  107.75 -87.00-168.46  158
 13  \w     36.00 112.00   0.50    6.00    --  107.75 -40.00  37.17  152
 14  \w     62.00 176.00   0.50    6.00    --  107.75  12.00-117.53  228
 15  \w     39.00 117.00   0.50    6.00    --  107.75 -54.00 170.84  156
 16  \w     37.00 114.00   0.50    6.00    --  107.75 -29.00 -55.49  154
 17  \w     39.00 141.00   0.50    6.00    --  107.75 -13.00 -12.03  204
 18  \w     49.00 126.00   0.50    1.00    --   62.00  71.00-105.58  154
 19  \w     63.00 141.00   0.50    1.00    --   74.00  62.00  22.27  156
 20  \w     69.00 147.00   0.50    1.00    --   78.00  51.00 -29.96  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1255097000
_diffrn_orient_matrix_UB_12      0.0522860000
_diffrn_orient_matrix_UB_13      -0.0966687000
_diffrn_orient_matrix_UB_21      0.1538460000
_diffrn_orient_matrix_UB_22      0.0998819000
_diffrn_orient_matrix_UB_23      -0.0130802000
_diffrn_orient_matrix_UB_31      0.0897442000
_diffrn_orient_matrix_UB_32      -0.0982581000
_diffrn_orient_matrix_UB_33      -0.0648555000
_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  0.0232
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10532
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.071
_diffrn_reflns_theta_min         5.455
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.808
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0514P)^2^+0.3327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1878
_reflns_number_total             2060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-187b-meoh_abs_2
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_database_code               7248788
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H14 N6 O6'
_chemical_oxdiff_usercomment     'pale block'
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C8(H8), C11(H11), C10(H10), C9(H9), C5(H5), C4(H4)
;
_shelx_res_checksum              14913
_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 0.848