A dinuclear phosphite rhodium(I) complex obtained by syngas treatment of a Rh/hydroxy phosphonite olefin hydroformylation precatalyst
Selent, Detlef; Spannenberg, Anke; Kubis, Christoph; Börner, Armin; Acta Crystallographica Section C 75 (2019) 398–401; doi:10.1107/S2053229619002730

data_2021528
_publ_section_title
;
 A dinuclear phosphite rhodium(I) complex obtained by syngas treatment of
 a Rh/hydroxy phosphonite olefin hydroformylation precatalyst
;
_journal_coeditor_code           QF3023
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              398
_journal_page_last               401
_journal_paper_doi               10.1107/S2053229619002730
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Rh2 (C22 H28 O5 P1)2 (C34 H37 O5 P1)2 (C O)2], 4C7 H8'
_chemical_formula_moiety         'C114 H130 O22 P4 Rh2, 4(C7 H8)'
_chemical_formula_sum            'C142 H162 O22 P4 Rh2'
_chemical_formula_weight         2550.41
_chemical_name_systematic
;
Bis[\m-(4,8-di-<i>tert</i>-butyl-2,10-dimethoxydibenzo[<i>d</i>,<i>f</i>]\
[1,3,2]dioxaphosphepin-6-yl)oxy]-1:2\k^2^<i>P</i>:\
<i>O</i>;\
1:2\k^2^<i>O</i>:<i>P</i>-bis{[6-([1,1'-biphenyl]-2-yloxy)-4,8-di-<i>tert</i>-\
butyl-2,10-dimethoxydibenzo[<i>d</i>,<i>f</i>][1,3,2]dioxaphosphepine-\
\k<i>P</i>]carbonylrhodium} toluene tatrasolvate
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.7430(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4100(5)
_cell_length_b                   15.5455(5)
_cell_length_c                   31.1570(11)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.28
_cell_measurement_theta_min      2.28
_cell_volume                     6419.7(4)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (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 APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            140325
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.578
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.336
_exptl_crystal_size_min          0.324
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         15481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+5.3591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                13358
_reflns_number_total             15481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qf3023sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2021528.cif.'
_cod_database_code               2021528
_cod_database_fobs_code          2021528
_shelx_hkl_checksum              80805
_shelx_res_checksum              15250