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_7242026
_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 H42 Na4 O14, 2(H2 O), 0.25(O)'
_chemical_formula_sum            'C50 H46.5 Na4 O16.25'
_chemical_formula_weight         999.33
_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             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                 96.564(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.8138(11)
_cell_length_b                   7.9496(4)
_cell_length_c                   26.0910(11)
_cell_measurement_reflns_used    14348
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      27.2640
_cell_measurement_theta_min      3.5130
_cell_volume                     4700.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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(14)
_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 0.943
_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    -25.00  61.00   1.00   45.00    --   18.95 -99.00-120.00   86
  2  \w    -25.00  61.00   1.00   45.00    --   18.95 -99.00  60.00   86
  3  \w    -54.00  45.00   1.00   45.00    --   18.95 -37.00  90.00   99
  4  \w    -25.00  22.00   1.00   45.00    --  -19.50 -99.00  90.00   47
  5  \w    -41.00  49.00   1.00   45.00    --  -19.50  57.00 -30.00   90
  6  \w    -92.00   6.00   1.00   45.00    --  -19.50 -37.00 -60.00   98
  7  \w    -90.00  11.00   1.00   45.00    --  -19.50 -77.00-120.00  101
  8  \w    -88.00   2.00   1.00   45.00    --  -19.50 -57.00 150.00   90
  9  \w    -92.00   6.00   1.00   45.00    --  -19.50 -37.00  30.00   98
 10  \w    -25.00  61.00   1.00   45.00    --   18.95 -99.00 -60.00   86
 11  \w     32.00  96.00   1.00   45.00    --   18.95-178.00 150.00   64
 12  \w    -25.00  61.00   1.00   45.00    --   18.95 -99.00  30.00   86
 13  \w     -9.00  72.00   1.00   45.00    --   18.95-118.00 -14.00   81
 14  \w    -90.00  11.00   1.00   45.00    --  -19.50 -77.00  90.00  101
 15  \w    -72.00   9.00   1.00   45.00    --  -19.50 118.00  71.00   81
 16  \w    -25.00  22.00   1.00   45.00    --  -19.50 -99.00 -60.00   47
 17  \w    -54.00  92.00   1.00   45.00    --   18.95   0.00-150.00  146
 18  \w    -54.00  44.00   1.00   45.00    --   18.95   0.00-120.00   98
 19  \w    -54.00  92.00   1.00   45.00    --   18.95   0.00-180.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0121681000
_diffrn_orient_matrix_UB_12      0.0038104000
_diffrn_orient_matrix_UB_13      0.0238039000
_diffrn_orient_matrix_UB_21      0.0283569000
_diffrn_orient_matrix_UB_22      0.0178132000
_diffrn_orient_matrix_UB_23      0.0129931000
_diffrn_orient_matrix_UB_31      -0.0052484000
_diffrn_orient_matrix_UB_32      0.0873259000
_diffrn_orient_matrix_UB_33      -0.0036814000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1544
_diffrn_reflns_av_unetI/netI     0.1193
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            159057
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.361
_diffrn_reflns_theta_min         3.373
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.412
_exptl_crystal_description       rod
_exptl_crystal_F_000             2082
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         12168
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0628P)^2^+1.5122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6829
_reflns_number_total             12168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01505a3.cif
_cod_data_source_block           '[Na(TBAPy)](acetone)'
_cod_original_formula_sum        'C50 H46.50 Na4 O16.25'
_cod_database_code               7242026
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C25H30O4Na1
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.948
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All C(H,H,H,H,H,H) groups, All O(H,H) groups, All O(H,
  H,H,H) groups
2. Restrained distances
 C71-C73
 1.45 with sigma of 0.02
 O64-H64B
 -0.95 with sigma of 0.02
 O64-H64A
 -0.95 with sigma of 0.02
 O61-H61B
 -0.95 with sigma of 0.02
 O61-H61A
 -0.95 with sigma of 0.02
 O62-H62B
 -0.95 with sigma of 0.02
 O62-H62A
 -0.95 with sigma of 0.02
 O63-H63A
 -0.95 with sigma of 0.02
 O63-H63B
 -0.95 with sigma of 0.02
 O81-H81A
 -0.95 with sigma of 0.02
 O81-H81B
 -0.95 with sigma of 0.02
 O80-H80B
 1.05 with sigma of 0.02
 O80-H80A
 1.05 with sigma of 0.02
 C71-C72
 1.45 with sigma of 0.02
 C71-C72B
 -1.4 with sigma of 0.02
 O70-C71
 -1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O70 \\sim C71 \\sim C72 \\sim C73: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C72) = Uanis(C72B)
4. Others
 Sof(C72B)=Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(C73B)=Sof(H73D)=Sof(H73E)=
 Sof(H73F)=1-FVAR(1)
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=
 FVAR(1)
 Fixed Sof: O82(0.25)
5.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)
5.b Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C72B(H72D,H72E,H72F), C73(H73A,H73B,H73C), C73B(H73D,
 H73E,H73F), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C)
;
_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 1.096
_oxdiff_exptl_absorpt_empirical_full_min 0.876