Photochemical H<sub>2</sub> activation by an Zn-Fe heterometallic: a mechanistic investigation.
Perez-Jimenez, Marina; Crimmin, Mark R.; Chemical science 15 (2024) 1424–1430; doi:10.1039/d3sc05966a

data_1570556
_publ_section_title
;
 Photochemical H<sub>2</sub> activation by an Zn-Fe heterometallic: a
 mechanistic investigation.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1424
_journal_page_last               1430
_journal_paper_doi               10.1039/d3sc05966a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C30 H34 Fe N2 O2 Zn'
_chemical_formula_sum            'C30 H34 Fe N2 O2 Zn'
_chemical_formula_weight         575.81
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-08-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-09-25 deposited with the CCDC.	2023-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1876(4)
_cell_length_b                   14.5939(3)
_cell_length_c                   26.9748(5)
_cell_measurement_reflns_used    3291
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      73.3700
_cell_measurement_theta_min      4.5050
_cell_volume                     5585.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.960
_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    -30.00  70.00   1.00    2.88    --   42.36 -57.00 150.00  100
  2  \w     52.00 128.00   1.00   15.24    --  105.75 -77.00 120.00   76
  3  \w     33.00 126.00   1.00   15.24    --  105.75 -61.00 -30.00   93
  4  \w     82.00 132.00   1.00   15.24    --  105.75 -45.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0165596000
_diffrn_orient_matrix_UB_12      -0.1019869000
_diffrn_orient_matrix_UB_13      -0.0119397000
_diffrn_orient_matrix_UB_21      0.0838210000
_diffrn_orient_matrix_UB_22      0.0015102000
_diffrn_orient_matrix_UB_23      -0.0362710000
_diffrn_orient_matrix_UB_31      0.0669109000
_diffrn_orient_matrix_UB_32      -0.0273365000
_diffrn_orient_matrix_UB_33      0.0424801000
_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  0.0482
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10742
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.663
_diffrn_reflns_theta_min         4.523
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.438
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0266P)^2^+2.1980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4218
_reflns_number_total             5419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05966a3.cif
_cod_data_source_block           mrc2370
_cod_depositor_comments
'Adding full bibliography for 1570556--1570557.cif.'
_cod_database_code               1570556
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C50 H120 N2 O2 Zn1 Fe1'
_chemical_oxdiff_usercomment     MPJ-161
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.586
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C19(H19), C17(H17), C28(H28), C8(H8), C10(H10), C27(H27), C26(H26),
 C25(H25), C24(H24)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C21(H21A,H21B,H21C),
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C13(H13A,H13B,
 H13C)
;
_shelx_res_checksum              73422
_shelx_hkl_checksum              4843
_olex2_date_sample_data_collection 2023-06-27
_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 1.169
_oxdiff_exptl_absorpt_empirical_full_min 0.895