Carbonyl{3,3'-di-<i>tert</i>-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-tetramethyl-1,3,2-dioxaphospholan-2-yl)oxy]biphenyl-κ^2^<i>P</i>,<i>P</i>'}hydrido(triphenylphosphane-κ<i>P</i>)rhodium(I) diethyl ether trisolvate
Selent, Detlef; Spannenberg, Anke; Börner, Armin; Acta Crystallographica Section E 69 (2013) m14–; doi:10.1107/S1600536812049124

data_2237243
_publ_section_title
;
 Carbonyl{3,3'-di-<i>tert</i>-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-tetramethyl-1,3,2-dioxaphospholan-2-yl)oxy]biphenyl-\k^2^<i>P</i>,<i>P</i>'}hydrido(triphenylphosphane-\k<i>P</i>)rhodium(I)
 diethyl ether trisolvate
;
_journal_coeditor_code           WM2697
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m14
_journal_paper_doi               10.1107/S1600536812049124
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'[Rh H (C74 H68 O8 P2) (C18 H15 P) (C O)], 3C4 H10 O'
_chemical_formula_moiety         'C93 H84 O9 P3 Rh, 3 (C4 H10 O)'
_chemical_formula_sum            'C105 H114 O12 P3 Rh'
_chemical_formula_weight         1763.78
_chemical_name_systematic
;
Carbonyl{3,3'-di-<i>tert</i>-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-
tetramethyl-1,3,2-dioxaphospholan-2-yl)oxy]biphenyl-
\k^2^<i>P</i>,<i>P</i>'}hydrido(triphenylphosphane-\k<i>P</i>)rhodium(I)
diethyl ether trisolvate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                112.3450(10)
_cell_angle_beta                 101.1350(10)
_cell_angle_gamma                96.7570(10)
_cell_formula_units_Z            4
_cell_length_a                   21.1611(4)
_cell_length_b                   22.1298(4)
_cell_length_c                   22.6020(4)
_cell_measurement_reflns_used    9259
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.25
_cell_volume                     9389.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_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 Kappa APEXII DUO'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            388867
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
Contributions of further disordered solvent molecules were removed
from the diffraction data with PLATON / SQUEEZE (Spek, 2009).
;
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.992
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1866
_refine_ls_number_reflns         43155
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+5.5129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                32017
_reflns_number_total             43155
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2697.cif
_cod_data_source_block           I
_cod_database_code               2237243
_cod_database_fobs_code          2237243