Photocatalytic turnover of CO2 under visible light by [Re(CO)3(1-(1,10) phenanthroline-5-(4-nitro-naphthalimide))Cl] in tandem with the sacrificial donor BIH
Spear, Alyssa; Schuarca, Robson L.; Bond, Jesse Q.; Korter, Timothy M.; Zubieta, Jon; Doyle, Robert P.; RSC Advances 12 (2022) 5080–5084; doi:10.1039/D1RA08261B

data_7244388
_publ_section_title
;
 Photocatalytic turnover of CO2 under visible light by [Re(CO)3(1-(1,10)
 phenanthroline-5-(4-nitro-naphthalimide))Cl] in tandem with the
 sacrificial donor BIH
;
_journal_issue                   9
_journal_name_full               'RSC Advances'
_journal_page_first              5080
_journal_page_last               5084
_journal_paper_doi               10.1039/D1RA08261B
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C27 H12 Br0.796 Cl0.204 N4 O7 Re, C7 H8'
_chemical_formula_sum            'C34 H20 Br0.8 Cl0.2 N4 O7 Re'
_chemical_formula_weight         853.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-27
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-05-28 deposited with the CCDC.	2022-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                107.983(2)
_cell_angle_beta                 95.125(2)
_cell_angle_gamma                96.9490(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4778(2)
_cell_length_b                   13.3551(2)
_cell_length_c                   13.9955(3)
_cell_measurement_reflns_used    29783
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1740
_cell_measurement_theta_min      3.3330
_cell_volume                     1482.59(6)
_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-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_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     29.00 122.00   0.50    0.07    --   49.62  77.00 150.00  186
  2  \w     29.00 112.00   0.50    0.07    --   49.62  77.00 -30.00  166
  3  \w     29.00 122.00   0.50    0.07    --   49.62  77.00 -60.00  186
  4  \w     29.00 122.00   0.50    0.07    --   49.62  77.00-120.00  186
  5  \w     37.00 122.00   0.50    0.07    --   49.62  57.00-150.00  170
  6  \w    -23.00   5.00   0.50    0.07    --   49.62 -19.00-120.00   56
  7  \w     34.00  87.00   0.50    0.30    --  105.75 -61.00-120.00  106
  8  \w     34.00 127.00   0.50    0.30    --  105.75 -77.00-120.00  186
  9  \w     34.00  87.00   0.50    0.30    --  105.75 -61.00 -90.00  106
 10  \w     34.00 127.00   0.50    0.30    --  105.75 -77.00  30.00  186
 11  \w     34.00  87.00   0.50    0.30    --  105.75 -61.00  30.00  106
 12  \w     34.00  87.00   0.50    0.30    --  105.75 -61.00 150.00  106
 13  \w    -23.00   5.00   0.50    0.07    --   49.62 -19.00 150.00   56
 14  \w    -23.00   5.00   0.50    0.07    --   49.62 -19.00  30.00   56
 15  \w     34.00  87.00   0.50    0.30    --  105.75 -61.00-150.00  106
 16  \w     34.00  87.00   0.50    0.30    --  105.75 -61.00-180.00  106
 17  \w     50.00 118.00   0.50    0.07    --   49.62-161.00-100.00  136
 18  \w     50.00 141.00   0.50    0.30    --  105.75-161.00-100.00  182
 19  \w     38.00 125.00   0.50    0.30    --  105.75-136.00-108.23  174
 20  \w     34.00 116.00   0.50    0.30    --  105.75-125.00-120.00  164
 21  \w     42.00 131.00   0.50    0.30    --  105.75-144.00 -60.30  178
 22  \w     34.00 116.00   0.50    0.30    --  105.75-125.00  30.00  164
 23  \w     34.00 116.00   0.50    0.30    --  105.75-125.00  60.00  164
 24  \w     34.00 116.00   0.50    0.30    --  105.75-125.00 120.00  164
 25  \w     34.00 116.00   0.50    0.30    --  105.75-125.00 150.00  164
 26  \w     44.00 133.00   0.50    0.30    --  105.75-148.00 104.79  178
 27  \w     34.00 112.00   0.50    0.30    --  105.75-117.00  50.00  156
 28  \w     34.00 109.00   0.50    0.30    --  105.75 -94.00 120.00  150
 29  \w     26.00  91.00   0.50    0.07    --   49.62-117.00  50.00  130
 30  \w     34.00 116.00   0.50    0.30    --  105.75-125.00-180.00  164
 31  \w     34.00 109.00   0.50    0.30    --  105.75 -94.00-120.00  150
 32  \w     97.00 178.00   0.50    0.30    --  105.75 117.00 137.00  162
 33  \w     92.00 178.00   0.50    0.30    --  105.75 125.00  60.00  172
 34  \w     68.00 122.00   0.50    0.07    --   49.62 161.00 -72.00  108
 35  \w     68.00 163.00   0.50    0.30    --  105.75 161.00 -72.00  190
 36  \w     92.00 178.00   0.50    0.30    --  105.75 125.00 -90.00  172
 37  \w     85.00 178.00   0.50    0.30    --  105.75  77.00  90.00  186
 38  \w     92.00 178.00   0.50    0.30    --  105.75  61.00 120.00  172
 39  \w     85.00 178.00   0.50    0.30    --  105.75  77.00  30.00  186
 40  \w     97.00 178.00   0.50    0.30    --  105.75  45.00  60.00  162
 41  \w     98.00 164.00   0.50    0.30    --  105.75  15.00 120.00  132
 42  \w     98.00 164.00   0.50    0.30    --  105.75  15.00-120.00  132
 43  \w     98.00 164.00   0.50    0.30    --  105.75  15.00-150.00  132
 44  \w    -42.00 -12.00   0.50    0.30    --  -84.25  45.00 -30.00   60
 45  \w   -116.00 -28.00   0.50    0.07    --  -49.62 161.00 -72.00  176
 46  \w   -115.00 -28.00   0.50    0.30    --  -84.25 161.00 -72.00  174
 47  \w    -87.00 -12.00   0.50    0.30    --  -84.25 117.00 137.00  150
 48  \w    -87.00  -4.00   0.50    0.07    --  -49.62 117.00 137.00  166
 49  \w   -121.00 -37.00   0.50    0.07    --  -49.62 -57.00  60.00  168
 50  \w   -121.00 -37.00   0.50    0.07    --  -49.62 -57.00 150.00  168
 51  \w   -121.00 -29.00   0.50    0.07    --  -49.62 -77.00 120.00  184
 52  \w   -121.00 -29.00   0.50    0.07    --  -49.62 -77.00  30.00  184
 53  \w   -121.00 -29.00   0.50    0.07    --  -49.62 -77.00   0.00  184
 54  \w   -121.00 -37.00   0.50    0.07    --  -49.62 -57.00-150.00  168
 55  \w   -121.00 -37.00   0.50    0.07    --  -49.62 -57.00 -90.00  168
 56  \w   -121.00 -75.00   0.50    0.07    --  -49.62-117.00  50.00   92
 57  \w   -121.00 -70.00   0.50    0.07    --  -49.62-125.00  90.00  102
 58  \w   -121.00 -70.00   0.50    0.07    --  -49.62-125.00 -60.00  102
 59  \w   -121.00 -46.00   0.50    0.07    --  -49.62-161.00-100.00  150
 60  \w   -146.00 -46.00   0.50    0.30    --  -84.25-161.00-100.00  200
 61  \w   -156.00 -75.00   0.50    0.30    --  -84.25-117.00  50.00  162
;
_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      0.1131932000
_diffrn_orient_matrix_UB_12      -0.0801252000
_diffrn_orient_matrix_UB_13      0.0071433000
_diffrn_orient_matrix_UB_21      0.0034268000
_diffrn_orient_matrix_UB_22      -0.0322889000
_diffrn_orient_matrix_UB_23      -0.1153176000
_diffrn_orient_matrix_UB_31      0.1459509000
_diffrn_orient_matrix_UB_32      0.0872732000
_diffrn_orient_matrix_UB_33      0.0170016000
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50161
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.951
_diffrn_reflns_theta_min         3.350
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.949
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54834
_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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       needle
_exptl_crystal_F_000             829
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.673
_refine_diff_density_min         -2.216
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         6228
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0538P)^2^+8.3150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5962
_reflns_number_total             6228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08261b2.cif
_cod_data_source_block           syras01
_cod_original_cell_volume        1482.59(5)
_cod_original_formula_sum        'C34 H20 Br0.80 Cl0.20 N4 O7 Re'
_cod_database_code               7244388
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.319
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 Re1-Br1
 2.56 with sigma of 0.02
 Re1-Cl1
 2.41 with sigma of 0.02
3. Restrained planarity
 C28, C29, C30, C31, C32, C33, C34
 with sigma of 0.04
 C28', C29', C30', C31', C32', C33', C34'
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
Uanis(Br1) = Uanis(Cl1)
5. Rigid body (RIGU) restrains
 C28, C29, C30, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28', C29', C30', C31', C32', C33', C34'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C28, C29, C34, C33, C32, C31, C30} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C28, C29, C30, C31, C32, C33, C34}
{C28', C29', C34', C33', C32', C31', C30'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C28', C29', C30', C31', C32', C33', C34'}
7. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(Br1)=FVAR(1)
 Sof(C28')=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29')=Sof(C30')=Sof(H30')=
 Sof(C31')=Sof(H31')=Sof(C32')=Sof(H32')=Sof(C33')=Sof(H33')=Sof(C34')=
 Sof(H34')=1-FVAR(2)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(C30)=Sof(H30)=Sof(C31)=
 Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C11(H11), C12(H12), C13(H13), C21(H21),
 C22(H22), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C30'(H30'), C31'(H31'), C32'(H32'), C33'(H33'), C34'(H34')
8.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C28'(H28D,H28E,H28F)
;
_shelx_res_checksum              23558
_olex2_submission_original_sample_id syras01
_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 2.335
_oxdiff_exptl_absorpt_empirical_full_min 0.527