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_7248787
_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 H36 Cu2 N10 O8, 4(H2 O)'
_chemical_formula_sum            'C56 H44 Cu2 N10 O12'
_chemical_formula_weight         1176.09
_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             2023-11-20
_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                111.044(2)
_cell_angle_beta                 107.145(2)
_cell_angle_gamma                95.432(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8808(3)
_cell_length_b                   11.1603(3)
_cell_length_c                   12.5136(3)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      78.3890
_cell_measurement_theta_min      4.3490
_cell_volume                     1320.49(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_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 0.979
_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     -4.00  79.00   0.50    5.00    --   52.54 -92.00  97.00  166
  2  \w     46.00 105.00   0.50   19.00    --  101.90 -92.00  97.00  118
  3  \w    102.00 158.00   0.50   19.00    --  101.90  92.00-150.00  112
  4  \w    -37.00  -9.00   0.50    5.00    --    6.00 120.00  93.38   56
  5  \w     -9.00  43.00   0.50    5.00    --   14.00  88.00  11.60  104
  6  \w      4.00  41.00   0.50    5.00    --   30.00  92.00 -68.33   74
  7  \w     16.00  43.00   0.50    5.00    --   34.00  79.00-143.24   54
  8  \w     -3.00  79.00   0.50    5.00    --   52.75 -92.00  97.00  164
  9  \w     54.00 132.00   0.50    5.00    --   70.00  76.00-171.13  156
 10  \w     59.00 137.00   0.50    5.00    --   70.00  60.00 -86.90  156
 11  \w     43.00 106.00   0.50   19.00    --  101.90 -99.00-150.00  126
 12  \w     34.00 112.00   0.50   19.00    --  101.90 -57.00  60.00  156
 13  \w     43.00 106.00   0.50   19.00    --  101.90 -99.00   0.00  126
 14  \w     95.00 166.00   0.50   19.00    --  101.90 125.00 150.00  142
 15  \w     32.00 120.00   0.50   19.00    --  101.90 -19.00-120.00  176
 16  \w     43.00 106.00   0.50   19.00    --  101.90 -99.00 -90.00  126
 17  \w     53.00 132.00   0.50   19.00    --  107.75 -88.00  49.89  158
 18  \w     43.00 163.00   0.50   19.00    --  107.75  -7.00-115.48  240
 19  \w     96.00 178.00   0.50   19.00    --  107.75  25.00  82.93  164
 20  \w     52.00 131.00   0.50   19.00    --  107.75 -87.00 -54.84  158
 21  \w     51.00 130.00   0.50   19.00    --  107.75 -86.00 154.51  158
 22  \w     38.00 125.00   0.50   19.00    --  107.75 -20.00-150.48  174
 23  \w     46.00 123.00   0.50   19.00    --  107.75 -75.00-162.50  154
 24  \w     38.00 115.00   0.50   19.00    --  107.75 -46.00-128.82  154
 25  \w     38.00 116.00   0.50   19.00    --  107.75 -47.00  -3.33  156
 26  \w     37.00 114.00   0.50   19.00    --  107.75 -44.00 -74.60  154
 27  \w     47.00 125.00   0.50   19.00    --  107.75 -78.00 -33.37  156
 28  \w     36.00 112.00   0.50   19.00    --  107.75 -40.00 145.67  152
 29  \w     37.00 121.00   0.50   19.00    --  107.75 -23.00  49.05  168
 30  \w     14.00  43.00   0.50    5.00    --   38.00  89.00 129.67   58
 31  \w     66.00 144.00   0.50    5.00    --   74.00  47.00  17.28  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      -0.1221169000
_diffrn_orient_matrix_UB_12      -0.0772646000
_diffrn_orient_matrix_UB_13      -0.1165385000
_diffrn_orient_matrix_UB_21      -0.0848680000
_diffrn_orient_matrix_UB_22      0.0866182000
_diffrn_orient_matrix_UB_23      0.0579449000
_diffrn_orient_matrix_UB_31      0.0317471000
_diffrn_orient_matrix_UB_32      0.0978163000
_diffrn_orient_matrix_UB_33      -0.0543300000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21942
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.519
_diffrn_reflns_theta_min         4.047
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.916
_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            'bluish green'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.061
_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     389
_refine_ls_number_reflns         5597
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0504P)^2^+1.2960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4924
_reflns_number_total             5597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-150-blue2_abs_2
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_original_cell_volume        1320.49(6)
_cod_database_code               7248787
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H20 N6 O6 Cu1'
_chemical_oxdiff_usercomment     'blue green block'
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.865
_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. Restrained distances
 N38B-C37
 1.34 with sigma of 0.02
3. Others
 Fixed Sof: N6(0.5) H6A(0.5) H6B(0.5) N38B(0.25) H38A(0.25) H38B(0.25)
 N38A(0.25) H38C(0.25) H38D(0.25)
4.a Free rotating group:
 O40(H40A,H40B), O39(H39A,H39B)
4.b Rotating group:
 N6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C18(H18), C9(H9), C12(H12), C10(H10), C29(H29), C25(H25), C36(H36),
 C22(H22), C28(H28), C15(H15), C31(H31), C24(H24), C23(H23), C17(H17), C16(H16)
4.d X=CH2 refined with riding coordinates:
 N38B(H38A,H38B), N38A(H38C,H38D)
;
_shelx_res_checksum              37735
_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 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.789