Effector responsive hydroformylation catalysis
Bai, Shaotao; Sinha, Vivek; Kluwer, Sander; Linnebank, Pim; Dydio, Pawel; Lutz, Martin; Abiri, Zohar; de Bruin, Bas; Reek, Joost N. H.; Chemical Science  (2019) –; doi:10.1039/C9SC02558H

data_1551514
_publ_section_title
;
 Effector responsive hydroformylation catalysis
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02558H
_journal_year                    2019
_chemical_formula_moiety
'C120 H100 N8 O6 P4 Rh2, 2(C2 H3 O2), 5.4(C H2 Cl2)'
_chemical_formula_sum            'C129.4 H116.8 Cl10.8 N8 O10 P4 Rh2'
_chemical_formula_weight         2656.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-11-05 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                70.329(1)
_cell_angle_beta                 75.142(1)
_cell_angle_gamma                70.305(1)
_cell_formula_units_Z            1
_cell_length_a                   12.8064(2)
_cell_length_b                   15.7601(3)
_cell_length_c                   17.3674(2)
_cell_measurement_reflns_used    32447
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      1.63
_cell_volume                     3066.93(9)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Eval15, Twinabs'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47177
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         1.625
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.745557
_exptl_absorpt_correction_T_min  0.671996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS-2008/4
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             1363
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.336
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.102
_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     762
_refine_ls_number_reflns         14043
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0740P)^2^+4.4051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11254
_reflns_number_total             14043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02558h2.cif
_cod_data_source_block           l0008a
_cod_original_cell_volume        3066.94(9)
_cod_original_formula_sum        'C129.40 H116.80 Cl10.80 N8 O10 P4 Rh2'
_cod_database_code               1551514
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              6420