Structural modulation of the photophysical and electronic properties of pyrene-based 3D metal‒organic frameworks derived from s-block metals
Coleman, Christopher N.; Tapping, Patrick C.; Huxley, Michael T.; Kee, Tak W.; Huang, David M.; Doonan, Christian J.; Sumby, Christopher J.; CrystEngComm 23 (2021) 82–90; doi:10.1039/D0CE01505A

data_7242024
_publ_section_title
;
 Structural modulation of the photophysical and electronic properties of
 pyrene-based 3D metal--organic frameworks derived from s-block metals
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              82
_journal_page_last               90
_journal_paper_doi               10.1039/D0CE01505A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C50 H36 N2 Na4 O10'
_chemical_formula_sum            'C50 H36 N2 Na4 O10'
_chemical_formula_weight         916.77
_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             2020-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-02 deposited with the CCDC.	2020-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.887(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7180(13)
_cell_length_b                   7.8066(6)
_cell_length_c                   24.1817(17)
_cell_measurement_reflns_used    4081
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      19.6920
_cell_measurement_theta_min      3.6130
_cell_volume                     4099.4(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -25.00   61.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9482  -99.0000  -30.0000 86

  2 omega  -25.00   61.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9482  -99.0000  150.0000 86

  3 omega  -25.00   61.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9482  -99.0000 -120.0000 86

  4 omega  -88.00    2.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951  -57.0000  -30.0000 90

  5 omega  -41.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951   57.0000   60.0000 90

  6 omega  -88.00    2.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951  -57.0000 -120.0000 90

  7 omega  -92.00    6.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951  -37.0000   30.0000 98

  8 omega  -25.00   22.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951  -99.0000 -180.0000 47

  9 omega  -92.00    6.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951  -37.0000  120.0000 98

 10 omega  -25.00   61.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9482  -99.0000   30.0000 86

 11 omega  -64.00   53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951   19.0000    0.0000 117

 12 omega  -95.00  -35.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951 -178.0000   90.0000 60

 13 omega  -56.00   39.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951   88.0000   39.0000 95

 14 omega  -25.00   22.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951  -99.0000   90.0000 47

 15 omega  -41.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951   57.0000  120.0000 90

 16 omega  -64.00   53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951   19.0000 -150.0000 117

 17 omega  -54.00   32.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9482    0.0000 -180.0000 86

 18 omega  -88.00    2.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951  -57.0000  -90.0000 90

 19 omega  -41.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951   57.0000  -30.0000 90

 20 omega  -41.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4951   57.0000  -90.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0158649000
_diffrn_orient_matrix_UB_12      0.0149584000
_diffrn_orient_matrix_UB_13      -0.0249988000
_diffrn_orient_matrix_UB_21      0.0063897000
_diffrn_orient_matrix_UB_22      0.0851201000
_diffrn_orient_matrix_UB_23      0.0085977000
_diffrn_orient_matrix_UB_31      0.0278367000
_diffrn_orient_matrix_UB_32      -0.0279798000
_diffrn_orient_matrix_UB_33      0.0127114000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3294
_diffrn_reflns_av_unetI/netI     0.1651
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            115555
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.059
_diffrn_reflns_theta_min         3.237
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       needle
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         7259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.2167
_refine_ls_R_factor_gt           0.1321
_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^)+(0.1479P)^2^+27.8806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3476
_refine_ls_wR_factor_ref         0.3874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3815
_reflns_number_total             7259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01505a3.cif
_cod_data_source_block           '[Na(TBAPy)](DMF)_omit'
_cod_database_code               7242024
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C25H30N4O4Na1
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.973
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.01
_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
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16), C22(H22),
 C23(H23), C25(H25), C26(H26), C32(H32), C37(H37), C38(H38), C42(H42), C43(H43),
  C45(H45), C46(H46), C52(H52), C53(H53), C55(H55), C56(H56), C61(H61), C71(H71)
2.b Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C73(H73A,H73B,H73C), C74(H74A,H74B,
 H74C)
;
_olex2_submission_special_instructions 'No special instructions were received'