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_2021780
_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 (C7 H8) (C36 H28 O P2)] B F4'
_chemical_formula_moiety         'C43 H36 O P2 Rh +, B F4 -'
_chemical_formula_sum            'C43 H36 B F4 O P2 Rh'
_chemical_formula_weight         820.38
_chemical_name_systematic
;
{Bis[(2-diphenylphosphanyl)phenyl]
ether-\k^2^<i>P</i>,<i>P</i>'}(\h^4^-norbornadiene)rhodium(I)
tetrafluoridoborate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.7420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8106(3)
_cell_length_b                   18.0754(2)
_cell_length_c                   18.1455(2)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.55
_cell_volume                     7028.24(15)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2014)
;
_computing_publication_material
;
SHELXTL (Bruker, 2014) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_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'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.604
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            orange
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_exptl_crystal_description       'part of prism'
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_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.320
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_refine_diff_density_min         -1.295
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         13063
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0408P)^2^+20.3084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                11013
_reflns_number_total             13063
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_database_fobs_code          2021780
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.823
_shelx_hkl_checksum              57149
_shelx_res_checksum              87584