A series of anionic MOFs with cluster-based, pillared-layer and rod-spacer motifs: near-sunlight white-light emission and selective dye capture
Wang, Ce; Yin, Zheng; Cheng, Zhao; Ma, Wei-Min; Li, Xi-Yao; Hu, Xiao-Ting; Shi, Rong; Chen, Ao-Wei; Ma, Yang-Min; CrystEngComm 22 (2020) 878–887; doi:10.1039/C9CE01691K

data_7239872
_publ_section_title
;
 A series of anionic MOFs with cluster-based, pillared-layer and
 rod-spacer motifs: near-sunlight white-light emission and selective dye
 capture
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              878
_journal_page_last               887
_journal_paper_doi               10.1039/C9CE01691K
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C29 H12 Mn3 O19, C4 H12 N'
_chemical_formula_sum            'C33 H24 Mn3 N O19'
_chemical_formula_weight         903.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-02 deposited with the CCDC.	2020-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.2808(8)
_cell_length_b                   19.8399(4)
_cell_length_c                   18.1612(4)
_cell_measurement_reflns_used    12573
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.8040
_cell_measurement_theta_min      2.6430
_cell_volume                     12044.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.957
_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    -57.00  33.00   0.50   10.00    --  -43.80  42.00-105.00  180
  2  \w     48.00  73.00   0.50   10.00    --   43.80  42.00-105.00   50
  3  \w    105.00 138.00   0.50   20.00    --  111.75  42.00-105.00   66
  4  \w     88.00 177.00   0.50   20.00    --  111.75  30.00   0.00  178
  5  \w    103.00 135.00   0.50   20.00    --  111.75 -42.00 102.00   64
  6  \w     65.00  95.00   0.50   20.00    --  111.75 -94.00  30.00   60
  7  \w     82.00 115.00   0.50   20.00    --  111.75-125.00 -30.00   66
  8  \w     56.00 135.00   0.50   20.00    --  111.75 -30.00-120.00  158
  9  \w     38.00  78.00   0.50   20.00    --  111.75-125.00 -30.00   80
 10  \w     36.00  98.00   0.50   20.00    --  111.75 -42.00 102.00  124
 11  \w     31.00 152.00   0.50   20.00    --  111.75 -15.00 -30.00  242
 12  \w     60.00 106.00   0.50   10.00    --   43.80 178.00  30.00   92
 13  \w    -88.00 -63.00   0.50   20.00    --  -90.25  42.00-105.00   50
 14  \w    -94.00 -48.00   0.50   20.00    --  -90.25 125.00   0.00   92
 15  \w    -95.00 -41.00   0.50   20.00    --  -90.25 125.00 -90.00  108
 16  \w   -120.00 -27.00   0.50   10.00    --  -43.80 -42.00 102.00  186
 17  \w   -120.00 -80.00   0.50   20.00    --  -90.25 -42.00 102.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0234527000
_diffrn_orient_matrix_UB_12      0.0411461000
_diffrn_orient_matrix_UB_13      0.0477679000
_diffrn_orient_matrix_UB_21      0.0366255000
_diffrn_orient_matrix_UB_22      -0.0010315000
_diffrn_orient_matrix_UB_23      0.0667698000
_diffrn_orient_matrix_UB_31      0.0152121000
_diffrn_orient_matrix_UB_32      0.0658509000
_diffrn_orient_matrix_UB_33      -0.0288002000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34638
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.996
_diffrn_reflns_theta_min         2.644
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.996
_exptl_crystal_description       prism
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         12181
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0984
_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^)+(0.1847P)^2^+71.3239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2865
_refine_ls_wR_factor_ref         0.3008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9875
_reflns_number_total             12181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01691k2.cif
_cod_data_source_block           1_sq_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7239868--7239872.cif.'
_cod_database_code               7239872
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.406
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C26-O15 = C26-O16 = C22-C26
 1.35 with sigma of 0.01
 O15-O16
 2.2 with sigma of 0.01
 C22-O15 = C22-O16
 2.33 with sigma of 0.01
 C32-C33
 1.4 with sigma of 0.01
3. Restrained planarity
 O15, O16, C22, C26
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C33) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.005
Uanis(O19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C14(H14), C16(H16), C21(H21), C23(H23),
 C25(H25)
5.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              7841
_shelx_fab_checksum              98944
_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 1.317
_oxdiff_exptl_absorpt_empirical_full_min 0.853