From zero-dimensional metallomacrocycle to three-dimensional metal–organic frameworks mediated by solvent polarity: near-white light emissions and gas adsorption properties
Yin, Jia-Ling; Yan, Qing-Qing; Liu, Yu-Xin; Yong, Guo-Ping; CrystEngComm 25 (2023) 4435–4444; doi:10.1039/D3CE00476G

data_7246931
_publ_section_title
;
 From zero-dimensional metallomacrocycle to three-dimensional
 metal--organic frameworks mediated by solvent polarity: near-white light
 emissions and gas adsorption properties
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              4435
_journal_page_last               4444
_journal_paper_doi               10.1039/D3CE00476G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C28 H16 Mn N4 O4'
_chemical_formula_sum            'C28 H16 Mn N4 O4'
_chemical_formula_weight         527.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-11-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-27 deposited with the CCDC.	2023-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.143(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4539(13)
_cell_length_b                   25.379(2)
_cell_length_c                   10.1811(7)
_cell_measurement_reflns_used    882
_cell_measurement_temperature    104(6)
_cell_measurement_theta_max      69.6740
_cell_measurement_theta_min      3.8680
_cell_volume                     2921.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2169
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.953
_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   -105.00 -17.00   1.00    8.00    --  -41.76 -38.00 -90.00   88
  2  \w    -86.00  -6.00   1.00    8.00    --  -41.76 125.00  60.00   80
  3  \w     33.00 131.00   1.00   16.00    --  106.05 -77.00 -60.00   98
  4  \w    120.00 178.00   1.00   16.00    --  106.05 125.00 -30.00   58
  5  \w    118.00 178.00   1.00   16.00    --  106.05  77.00  30.00   60
  6  \w     40.00 132.00   1.00   16.00    --  106.05 -45.00  30.00   92
  7  \w    103.00 178.00   1.00   16.00    --  106.05  77.00 150.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0031762000
_diffrn_orient_matrix_UB_12      -0.0551080000
_diffrn_orient_matrix_UB_13      -0.0625269000
_diffrn_orient_matrix_UB_21      -0.1309552000
_diffrn_orient_matrix_UB_22      0.0057304000
_diffrn_orient_matrix_UB_23      -0.0629768000
_diffrn_orient_matrix_UB_31      0.0377634000
_diffrn_orient_matrix_UB_32      0.0246979000
_diffrn_orient_matrix_UB_33      -0.1249628000
_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  0.1265
_diffrn_reflns_av_unetI/netI     0.1779
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10128
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.975
_diffrn_reflns_theta_min         3.909
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.975
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.00053(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0925
_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^)+(0.0378P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2466
_reflns_number_total             5565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00476g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7246930--7246932.cif.'
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7246931
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c20h20o1Ni1
_shelx_estimated_absorpt_t_max   0.587
_shelx_estimated_absorpt_t_min   0.475
_reflns_odcompleteness_completeness 98.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C19(H19), C13(H13), C23(H23), C11(H11), C28(H28), C26(H26),
 C5(H5), C16(H16), C25(H25), C27(H27), C15(H15), C10(H10), C8(H8), C9(H9)
;
_shelx_res_checksum              79479
_shelx_hkl_checksum              53727
_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 3.341
_oxdiff_exptl_absorpt_empirical_full_min 0.340