Magnesium-porphyrin as an efficient photocatalyst for the transformation of CO2 to cyclic carbonates and oxazolidinones under ambient conditions
Meher, Sushanta Kumar; Nayak, Prakash; Dhala, Sasmita; Tripathy, Swetapadma; Venkatasubbaiah, Krishnan; Catalysis Science & Technology 14 (2024) 3125–3130; doi:10.1039/D4CY00246F

data_1571418
_publ_section_title
;
 Magnesium-porphyrin as an efficient photocatalyst for the transformation
 of CO2 to cyclic carbonates and oxazolidinones under ambient conditions
;
_journal_issue                   11
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3125
_journal_page_last               3130
_journal_paper_doi               10.1039/D4CY00246F
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C48 H38 Mg N4 O, 2[H2O]'
_chemical_formula_sum            'C48 H38 Mg N4 O'
_chemical_formula_weight         711.168
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-02 deposited with the CCDC.	2024-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.3360(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6518(2)
_cell_length_b                   9.34996(12)
_cell_length_c                   24.7713(3)
_cell_measurement_reflns_used    20243
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.4100
_cell_measurement_theta_min      3.6860
_cell_volume                     3942.77(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9759
_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    -76.00  13.00   0.50    8.34    --  -38.50 103.00 -42.00  178
  2  \w      8.00  88.00   0.50    8.34    --   49.56-103.00-145.00  160
  3  \w    104.00 177.00   0.50   39.75    --  107.46 103.00 -42.00  146
  4  \w     38.00 108.00   0.50   39.75    --  107.46-103.00-145.00  140
  5  \w   -101.00 -27.00   0.50    8.34    --  -38.50 -57.00-120.00  148
  6  \w    -42.00  28.00   0.50    8.34    --  -38.50  37.00-180.00  140
  7  \w   -105.00 -35.00   0.50    8.34    --  -38.50 -37.00 150.00  140
  8  \w    -13.00  61.00   0.50    8.34    --   49.56 -57.00  30.00  148
  9  \w     95.00 170.00   0.50   39.75    --  107.46  61.00 -60.00  150
 10  \w     39.00 111.00   0.50   39.75    --  107.46 -30.00   0.00  144
 11  \w    103.00 172.00   0.50   39.75    --  107.46  45.00  30.00  138
 12  \w     51.00 112.00   0.50   39.75    --  107.46 -45.00 120.00  122
 13  \w     39.00 103.00   0.50   39.75    --  107.46 -94.00-120.00  128
 14  \w     51.00  87.00   0.50   39.75    --  107.46-125.00   0.00   72
 15  \w     46.00 112.00   0.50   39.75    --  107.46 -45.00  60.00  132
 16  \w     49.00 112.00   0.50   39.75    --  107.46 -45.00-120.00  126
 17  \w    106.00 164.00   0.50   39.75    --  107.46  77.00 -90.00  116
 18  \w    104.00 174.00   0.50   39.75    --  107.46  15.00  90.00  140
 19  \w     40.00  66.00   0.50   39.75    --  107.46 -94.00 -60.00   52
 20  \w     59.00  85.00   0.50   39.75    --  107.46 -94.00-180.00   52
 21  \w     47.00  91.00   0.50   39.75    --  107.46 -45.00 -30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0726543000
_diffrn_orient_matrix_UB_12      0.0854329000
_diffrn_orient_matrix_UB_13      -0.0045818000
_diffrn_orient_matrix_UB_21      -0.0150758000
_diffrn_orient_matrix_UB_22      -0.0459663000
_diffrn_orient_matrix_UB_23      -0.0616685000
_diffrn_orient_matrix_UB_31      -0.0517452000
_diffrn_orient_matrix_UB_32      0.1332640000
_diffrn_orient_matrix_UB_33      -0.0182894000
_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  0.0296
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.9994
_diffrn_reflns_Laue_measured_fraction_max 0.9759
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32534
_diffrn_reflns_point_group_measured_fraction_full 0.9994
_diffrn_reflns_point_group_measured_fraction_max 0.9759
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         77.98
_diffrn_reflns_theta_min         3.70
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.52a (Rigaku Oxford Diffraction, 2022)
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    1.198
_exptl_crystal_description       plate
_exptl_crystal_F_000             1501.143
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.5441
_refine_diff_density_min         -0.3694
_refine_diff_density_rms         0.0467
_refine_ls_d_res_high            0.7882
_refine_ls_d_res_low             11.9446
_refine_ls_goodness_of_fit_ref   1.0418
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    79
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8227
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.0406
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+1.3526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                7161
_reflns_number_total             8227
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cy00246f2.cif
_cod_data_source_block           KV_SKM_POR_auto
_cod_depositor_comments          'Adding full bibliography for 1571418.cif.'
_cod_original_formula_sum        'C48 H38 Mg1 N4 O1'
_cod_database_code               1571418
_chemical_oxdiff_formula         'C H N O Mg'
_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 O(H,H) groups
2. Rigid body (RIGU) restrains
 C48B, C48A, C45B, C45A, C44B, C43B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: C44B(0.5) H44B(0.5) C43B(0.5) H43B(0.5) C46A(0.5) H46A(0.5)
 C42B(0.5) C47B(0.5) H47B(0.5) C42A(0.5) C45B(0.5) C47A(0.5) H47A(0.5)
 C46B(0.5) H46B(0.5) C43A(0.5) H43A(0.5) C44A(0.5) H44A(0.5) C48B(0.5)
 H48a(0.5) H48b(0.5) H48c(0.5) C48A(0.5) H48d(0.5) H48e(0.5) H48f(0.5)
 C45A(0.5) O4(0.4) O2(0.6) O5(0.45)
4.a Rotating group:
 O1(H1a,H1b)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C26(H26), C19(H19), C14(H14), C25(H25), C33(H33), C13(H13),
 C32(H32), C3(H3), C29(H29), C30(H30), C36(H36), C40(H40), C4(H4), C37(H37),
 C22(H22), C39(H39), C23(H23), C9(H9), C8(H8), C44B(H44B), C43B(H43B),
 C46A(H46A), C47B(H47B), C47A(H47A), C46B(H46B), C43A(H43A), C44A(H44A)
4.c Idealised Me refined as rotating group:
 C34(H34a,H34b,H34c), C27(H27a,H27b,H27c), C41(H41a,H41b,H41c), C48B(H48a,H48b,
 H48c), C48A(H48d,H48e,H48f)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 78 electrons were 
found in a volume of 222\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[H2O] per Formula Unit 
which account for 80 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.638
_oxdiff_exptl_absorpt_empirical_full_min 0.754