Dehydropolymerisation of methylamine borane using highly active rhodium(iii) bis(thiophosphinite) pincer complexes: catalytic and mechanistic insights
Hasche, Patrick; Haak, Julia; Anke, Felix; Kubis, Christoph; Baumann, Wolfgang; Drexler, Hans-Joachim; Jiao, Haijun; Beweries, Torsten; Catalysis Science & Technology 11 (2021) 3514–3526; doi:10.1039/D1CY00124H

data_1561513
_publ_section_title
;
 Dehydropolymerisation of methylamine borane using highly active
 rhodium(iii) bis(thiophosphinite) pincer complexes: catalytic and
 mechanistic insights
;
_journal_issue                   10
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3514
_journal_page_last               3526
_journal_paper_doi               10.1039/D1CY00124H
_journal_volume                  11
_journal_year                    2021
_chemical_formula_sum            'C23 H37 Cl N P2 Rh S2'
_chemical_formula_weight         591.95
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-01-16 deposited with the CCDC.	2021-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.4200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4250(7)
_cell_length_b                   8.8088(4)
_cell_length_c                   17.9270(7)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.10
_cell_measurement_theta_min      2.61
_cell_volume                     2669.89(19)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73849
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.283
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       'part of prism'
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0192
_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^)+(0.0278P)^2^+0.8025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5250
_reflns_number_total             5818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00124h2.cif
_cod_data_source_block           ax1735abs2
_cod_depositor_comments
'Adding full bibliography for 1561513--1561515.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1561513
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.662
_shelx_estimated_absorpt_t_max   0.885
_shelx_res_checksum              69435