Dicarbonyl{3,3'-di-<i>tert</i>-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-tetraphenyl-1,3,2-dioxaphospholan-2-yl)oxy-κ<i>P</i>]biphenyl}hydridorhodium(I) diethyl ether monosolvate
Selent, Detlef; Spannenberg, Anke; Börner, Armin; Acta Crystallographica Section E 68 (2012) m488–; doi:10.1107/S1600536812011786

data_2234127
_publ_section_title
;
 Dicarbonyl{3,3'-di-<i>tert</i>-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-tetraphenyl-1,3,2-dioxaphospholan-2-yl)oxy-\k<i>P</i>]biphenyl}hydridorhodium(I)
 diethyl ether monosolvate
;
_journal_coeditor_code           BT5848
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m488
_journal_paper_doi               10.1107/S1600536812011786
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Rh (C74 H68 O8 P2) H (C O)2], C4 H10 O'
_chemical_formula_moiety         'C76 H69 O10 P2 Rh, C4 H10 O'
_chemical_formula_sum            'C80 H79 O11 P2 Rh'
_chemical_formula_weight         1381.28
_chemical_name_systematic
;
Dicarbonyl{3,3'-di-<i>tert</i>-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-
tetraphenyl-1,3,2-dioxaphospholan-2-yl)oxy-\k<i>P</i>]biphenyl}hydridorhodium(I)
diethyl ether monosolvate
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.263(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1489(2)
_cell_length_b                   25.8458(4)
_cell_length_c                   12.5941(3)
_cell_measurement_reflns_used    15841
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      1.68
_cell_volume                     3404.43(12)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            59171
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.9589
_exptl_absorpt_correction_T_min  0.8354
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.465
_refine_ls_abs_structure_details 'Flack (1983), 7944 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.026(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         16262
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0377P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                14238
_reflns_number_total             16262
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5848.cif
_cod_data_source_block           I
_cod_original_cell_volume        3404.43(11)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2234127
_cod_database_fobs_code          2234127