Determination of accessibility and spatial distribution of chiral Rh diene complexes immobilized on SBA-15 via phosphine-based solid-state NMR probe molecules
Rieg, Carolin; Kirchhof, Manuel; Gugeler, Katrin; Beurer, Ann-Katrin; Stein, Lukas; Dirnberger, Klaus; Frey, Wolfgang; Bruckner, Johanna R.; Traa, Yvonne; Kästner, Johannes; Ludwigs, Sabine; Laschat, Sabine; Dyballa, Michael; Catalysis Science & Technology 13 (2023) 410–425; doi:10.1039/D2CY01578A

data_1567995
_publ_section_title
;
 Determination of accessibility and spatial distribution of chiral Rh
 diene complexes immobilized on SBA-15 via phosphine-based solid-state NMR
 probe molecules
;
_journal_issue                   2
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              410
_journal_page_last               425
_journal_paper_doi               10.1039/D2CY01578A
_journal_volume                  13
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H60 Cl N O3 P Rh, C H Cl3'
_chemical_formula_sum            'C45 H61 Cl4 N O3 P Rh'
_chemical_formula_weight         939.62
_chemical_name_systematic        'compound [RhCl(L1)(P(Ad)2(n-Bu))]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-08-08 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.654(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.862(2)
_cell_length_b                   19.566(4)
_cell_length_c                   12.200(2)
_cell_measurement_reflns_used    8546
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.437
_cell_measurement_theta_min      1.796
_cell_volume                     2409.8(8)
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.437
_diffrn_reflns_theta_min         1.796
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.7264
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       prism
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.137
_refine_diff_density_max         1.481
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 3558 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9910
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+0.1095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                8546
_reflns_number_total             9910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy01578a2.cif
_cod_data_source_block           s2867lm_sq
_cod_depositor_comments          'Adding full bibliography for 1567995.cif.'
_cod_original_cell_volume        2409.9(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1567995
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              4820
_shelx_fab_checksum              3882