Structural and Electronic Effects of X-ray Irradiation on Prototypical [M(COD)Cl]<sub>2</sub> Catalysts.
Fernando, Nathalie K.; Cairns, Andrew B.; Murray, Claire A.; Thompson, Amber L.; Dickerson, Joshua L.; Garman, Elspeth F.; Ahmed, Nayera; Ratcliff, Laura E.; Regoutz, Anna; The journal of physical chemistry. A 125 (2021) 7473–7488; doi:10.1021/acs.jpca.1c05759

data_1564537
_publ_section_title
;
 Structural and Electronic Effects of X-ray Irradiation on Prototypical
 [M(COD)Cl]<sub>2</sub> Catalysts.
;
_journal_issue                   34
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              7473
_journal_page_last               7488
_journal_paper_doi               10.1021/acs.jpca.1c05759
_journal_volume                  125
_journal_year                    2021
_chemical_formula_moiety         'C16 H24 Cl2 Ir2'
_chemical_formula_sum            'C16 H24 Cl2 Ir2'
_chemical_formula_weight         671.71
_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'
_symmetry_Int_Tables_number      61
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-06-28 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.18382(11)
_cell_length_b                   13.64566(9)
_cell_length_c                   16.30646(10)
_cell_measurement_reflns_used    14389
_cell_measurement_temperature    300.0(1)
_cell_measurement_theta_max      25.1160
_cell_measurement_theta_min      1.9360
_cell_volume                     3378.59(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.8679
_diffrn_measured_fraction_theta_max 0.8679
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f      0.00 300.00   0.20    0.20   0.00   0.00   0.00    --  1500
;
_diffrn_measurement_device       'I15 Diamond Light Source EH1'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0329417000
_diffrn_orient_matrix_UB_12      0.0346367000
_diffrn_orient_matrix_UB_13      -0.0019056000
_diffrn_orient_matrix_UB_21      -0.0133148000
_diffrn_orient_matrix_UB_22      -0.0186123000
_diffrn_orient_matrix_UB_23      -0.0372591000
_diffrn_orient_matrix_UB_31      -0.0282148000
_diffrn_orient_matrix_UB_32      -0.0316647000
_diffrn_orient_matrix_UB_33      0.0198215000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22799
_diffrn_reflns_theta_full        25.2373
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         2.29
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    14.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.6409
_exptl_crystal_description       'colourless block'
_exptl_crystal_F_000             2451.1917
_refine_diff_density_max         0.6978
_refine_diff_density_min         -1.0307
_refine_diff_density_rms         0.2335
_refine_ls_d_res_high            0.8079
_refine_ls_d_res_low             8.6166
_refine_ls_goodness_of_fit_ref   0.9526
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2917
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9526
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                2668
_reflns_number_total             2917
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jp1c05759_si_002.cif
_cod_data_source_block           023nkf19_01_
_cod_database_code               1564537
_chemical_oxdiff_formula         'C16 H24 Ir2 Cl2'
_reflns_odcompleteness_completeness 86.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C15(H15a,
 H15b), C16(H16a,H16b), C18(H18a,H18b), C19(H19a,H19b)
;
_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 1.459
_oxdiff_exptl_absorpt_empirical_full_min 0.827