Iron-Catalyzed H/D Exchange of Primary Silanes, Secondary Silanes, and Tertiary Siloxanes
Linford-Wood, Thomas G.; Mahon, Mary F.; Grayson, Matthew N.; Webster, Ruth L.; ACS Catalysis  (2022) 2979–2985; doi:10.1021/acscatal.2c00224

data_4519340
_publ_section_title
;
 Iron-Catalyzed H/D Exchange of Primary Silanes, Secondary Silanes, and
 Tertiary Siloxanes
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              2979
_journal_page_last               2985
_journal_paper_doi               10.1021/acscatal.2c00224
_journal_year                    2022
_chemical_formula_moiety         'C42 H50 Fe N4'
_chemical_formula_sum            'C42 H50 Fe N4'
_chemical_formula_weight         666.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.96820(10)
_cell_length_b                   17.6194(2)
_cell_length_c                   18.8246(2)
_cell_measurement_reflns_used    13351
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.4870
_cell_measurement_theta_min      4.7010
_cell_volume                     3622.24(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38573
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.584
_diffrn_reflns_theta_min         3.443
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.589
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.9024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6543
_reflns_number_total             7182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs2c00224_si_003.cif
_cod_data_source_block           s21rlw39
_cod_database_code               4519340
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.427
_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:
 C4(H4), C5(H5), C6(H6), C11(H11), C17(H17), C18(H18), C19(H19), C25(H25),
 C26(H26), C27(H27), C32(H32), C38(H38), C39(H39), C40(H40)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C42(H42A,
 H42B,H42C)
;
_shelx_res_checksum              55984
_shelx_hkl_checksum              92936
_olex2_submission_special_instructions 'No special instructions were received'