Two precatalysts for application in asymmetric homogeneous hydrogenation
Meißner, Antje; Pribbenow, Cornelia; Drexler, Hans-Joachim; Heller, Detlef; Acta Crystallographica Section C 70 (2014) 941–944; doi:10.1107/S205322961401910X

data_2019653
_publ_section_title
;
 Two precatalysts for application in asymmetric homogeneous hydrogenation
;
_journal_coeditor_code           EG3166
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              941
_journal_page_last               944
_journal_paper_doi               10.1107/S205322961401910X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Rh (C34 H36 P2) (C8 H12)] B F4 , C H2 Cl2'
_chemical_formula_moiety         'C42 H48 P2 Rh 1+, B F4-, (C H2 Cl2)'
_chemical_formula_sum            'C43 H50 B Cl2 F4 P2 Rh'
_chemical_formula_weight         889.39
_chemical_name_systematic
;[(1<i>R</i>,1'<i>R</i>,2<i>R</i>,2'<i>R</i>)-2,2'-Bis(diphenylphosphanyl)-1,1'-dicyclopentane][\h^4^-(<i>Z</i>,<i>Z</i>)-cycloocta-1,5-diene]rhodium(I)
tetrafluoroborate dichloromethane monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL2014
_cell_angle_alpha                90
_cell_angle_beta                 108.2650(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2285(2)
_cell_length_b                   13.9823(3)
_cell_length_c                   14.5131(4)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.43
_cell_measurement_theta_min      2.91
_cell_volume                     1971.06(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    '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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_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  0.0337
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            64265
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         2.075
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.7485
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'part of prism'
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.458
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4470 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.015(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9780
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0228P)^2^+0.6524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                9496
_reflns_number_total             9780
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3166sup1.cif
_cod_data_source_block           RhBICPcodBF4
_cod_depositor_comments
'Adding full bibliography for 2019652--2019653.cif.'
_cod_database_code               2019653
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_shelx_hkl_checksum              40801
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