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_7246930
_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         'C112 H80 Mn4 N16 O24, 2(H2 O)'
_chemical_formula_sum            'C112 H84 Mn4 N16 O26'
_chemical_formula_weight         2289.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-02-21
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.4550(14)
_cell_length_b                   36.5541(14)
_cell_length_c                   11.0255(2)
_cell_measurement_reflns_used    4274
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.5670
_cell_measurement_theta_min      4.1480
_cell_volume                     15095.4(9)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4337
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.961
_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    -70.00  31.00   0.50    6.00    --  -42.30  57.00 -30.00  202
  2  \w     34.00  85.00   0.50   12.00    --  105.52 -94.00-180.00  102
  3  \w     50.00 110.00   0.50   12.00    --  105.52-125.00  90.00  120
  4  \w     31.00 144.00   0.50   12.00    --  105.52 -15.00 -90.00  226
;
_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      0.0044690000
_diffrn_orient_matrix_UB_12      -0.0197364000
_diffrn_orient_matrix_UB_13      0.0363211000
_diffrn_orient_matrix_UB_21      0.0164590000
_diffrn_orient_matrix_UB_22      -0.0369060000
_diffrn_orient_matrix_UB_23      -0.0192885000
_diffrn_orient_matrix_UB_31      0.1386475000
_diffrn_orient_matrix_UB_32      0.0049719000
_diffrn_orient_matrix_UB_33      0.0010855000
_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  0.0770
_diffrn_reflns_av_unetI/netI     0.1117
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            30350
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.810
_diffrn_reflns_theta_min         4.180
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.158
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_correction_T_min  0.595
_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    1.008
_exptl_crystal_description       block
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         14708
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1248P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2529
_refine_ls_wR_factor_ref         0.2972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7377
_reflns_number_total             14708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00476g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7246930--7246932.cif.'
_cod_database_code               7246930
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         c20h20n2o2Mg1Cl1
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.600
_reflns_odcompleteness_completeness 98.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
2.a Free rotating group:
 O13(H13A,H13B)
2.b Rotating group:
 O5(H5A,H5B), O6(H6A,H6B), O11(H11A,H11B), O12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C48(H48), C50(H50), C36(H36), C21(H21), C55(H55), C34(H34),
 C39(H39), C42(H42), C12(H12), C61(H61), C41(H41), C46(H46), C53(H53), C44(H44),
  C13(H13), C32(H32), C45(H45), C30(H30), C3(H3), C16(H16), C59(H59), C54(H54),
 C14(H14), C28(H28), C31(H31), C25(H25), C60(H60), C8(H8), C24(H24), C26(H26),
 C5(H5), C9(H9), C10(H10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8252
_shelx_hkl_checksum              76435
_shelx_fab_checksum              68190
_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 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.585