High loading of Mn(ii)-metalated porphyrin in a MOF for photocatalytic CO<sub>2</sub> reduction in gas-solid conditions.
Qin, Jian-Hua; Xu, Peng; Huang, Ya-Dan; Xiao, Lu-Yao; Lu, Weiwei; Yang, Xiao-Gang; Ma, Lu-Fang; Zang, Shuang-Quan; Chemical communications (Cambridge, England) 57 (2021) 8468–8471; doi:10.1039/d1cc02847b

data_7128693
_publ_section_title
;
 High loading of Mn(ii)-metalated porphyrin in a MOF for photocatalytic
 CO<sub>2</sub> reduction in gas-solid conditions.
;
_journal_issue                   68
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8468
_journal_page_last               8471
_journal_paper_doi               10.1039/d1cc02847b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C48 H32 Mn2 N4 O12'
_chemical_formula_sum            'C48 H32 Mn2 N4 O12'
_chemical_formula_weight         966.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-27 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.085(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0571(5)
_cell_length_b                   17.3975(6)
_cell_length_c                   13.7185(5)
_cell_measurement_reflns_used    11565
_cell_measurement_temperature    293.24(10)
_cell_measurement_theta_max      27.7550
_cell_measurement_theta_min      3.7380
_cell_volume                     3223.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      air
_diffrn_ambient_temperature      293.24(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.915
_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    -81.00  13.00   1.00   17.50    --  -13.80 -77.00 -90.00   94
  2  \w    -62.00   6.00   1.00   17.50    --  -13.80 115.00-103.00   68
  3  \w    -20.00  25.00   1.00   17.50    --  -13.80 -99.00 150.00   45
  4  \w    -52.00  32.00   1.00   17.50    --   14.82 -57.00  30.00   84
  5  \w    -52.00  32.00   1.00   17.50    --   14.82 -57.00  60.00   84
  6  \w     -4.00  84.00   1.00   17.50    --   14.82  38.00-150.00   88
  7  \w    -20.00  25.00   1.00   17.50    --  -13.80 -99.00 -60.00   45
  8  \w    -81.00   3.00   1.00   17.50    --  -13.80 -57.00  30.00   84
  9  \w    -20.00  54.00   1.00   17.50    --   14.82 -99.00 150.00   74
 10  \w    -52.00  32.00   1.00   17.50    --   14.82 -57.00 -90.00   84
 11  \w    -52.00  32.00   1.00   17.50    --   14.82 -57.00-180.00   84
 12  \w    -20.00  54.00   1.00   17.50    --   14.82 -99.00-120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0202751000
_diffrn_orient_matrix_UB_12      -0.0338231000
_diffrn_orient_matrix_UB_13      0.0151068000
_diffrn_orient_matrix_UB_21      0.0174068000
_diffrn_orient_matrix_UB_22      -0.0217325000
_diffrn_orient_matrix_UB_23      -0.0352779000
_diffrn_orient_matrix_UB_31      0.0452116000
_diffrn_orient_matrix_UB_32      -0.0067945000
_diffrn_orient_matrix_UB_33      0.0377278000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31852
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.450
_diffrn_reflns_theta_min         3.673
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.996
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0719P)^2^+0.4422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2991
_reflns_number_total             3851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02847b2.cif
_cod_data_source_block           20190310-35_sq
_cod_depositor_comments          'Adding full bibliography for 7128693.cif.'
_cod_database_code               7128693
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C1H1O1N1Mn1
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O3-H3 = O4-H4
 0.87 with sigma of 0.02
3.a Fixed occupancy and ADP/Uiso:
 H3, H4
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11)
;
_shelx_res_checksum              21413
_shelx_hkl_checksum              32940
_shelx_fab_checksum              20913
_platon_squeeze_void_probe_radius 1.20
_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 1.736
_oxdiff_exptl_absorpt_empirical_full_min 0.678