Two precatalysts for application in propargylic CH activation
Möller, Saskia; Drexler, Hans-Joachim; Heller, Detlef; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S205322961901163X

data_2021781
_publ_section_title
;
 Two precatalysts for application in propargylic CH activation
;
_journal_coeditor_code           OV3130
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322961901163X
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Rh (C8 H12) (C36 H28 O P2)] B F4, C H2 Cl2'
_chemical_formula_moiety         'C44 H40 O P2 Rh +, B F4 -, C H2 Cl2'
_chemical_formula_sum            'C45 H42 B Cl2 F4 O P2 Rh'
_chemical_formula_weight         921.34
_chemical_name_systematic
;
{Bis[(2-diphenylphosphanyl)phenyl]
ether-\k^2^<i>P</i>,<i>P</i>'}[\h^4^-(<i>Z</i>,<i>Z</i>)-cycloocta-1,5-\
diene]rhodium(I) tetrafluoridoborate dichloromethane monosolvate
;
_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-2014
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_cell_angle_beta                 74.6950(10)
_cell_angle_gamma                72.2620(10)
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_cell_length_a                   11.3056(3)
_cell_length_b                   12.8231(4)
_cell_length_c                   14.6101(4)
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_cell_measurement_theta_min      2.16
_cell_volume                     1944.29(10)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
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APEX2 (Bruker, 2014)
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_computing_data_reduction
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SAINT (Bruker, 2013)
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_computing_molecular_graphics
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SHELXTL (Bruker, 2014)
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_computing_publication_material
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SHELXTL (Bruker, 2014) and publCIF (Westrip, 2010)
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_computing_structure_refinement
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SHELXL2014 (Sheldrick, 2015)
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_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_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_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
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_diffrn_reflns_av_unetI/netI     0.0238
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_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.669
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_exptl_absorpt_correction_T_max  0.996
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
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_exptl_crystal_description       rod
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_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.115
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_refine_diff_density_min         -1.062
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_refine_ls_number_reflns         7240
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0636P)^2^+6.1906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1274
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_database_fobs_code          2021781
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.922
_shelx_hkl_checksum              79519
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